# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Allan Blackman' _publ_contact_author_email BLACKMAN@ALKALI.OTAGO.AC.NZ _publ_section_title ; The donor ability of the chelated carbonate ligand: protonation and metallation of [(L)Co(O2CO)]+ complexes in aqueous solution. ; loop_ _publ_author_name 'Allan Blackman' 'German Cavigliasso' 'Lisa F. McClintock' 'Rob Stranger' # Attachment 'Final_Structures.cif' data_lmzn2 _database_code_depnum_ccdc_archive 'CCDC 686136' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H22 Cl3 Co N4 O4 Zn' _chemical_formula_weight 613.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2809(8) _cell_length_b 11.2581(10) _cell_length_c 13.7533(11) _cell_angle_alpha 95.303(4) _cell_angle_beta 103.086(4) _cell_angle_gamma 107.175(5) _cell_volume 1175.59(18) _cell_formula_units_Z 2 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 5709 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 32.77 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 2.102 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.836884 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 85(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa ApexII area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 26030 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 33.34 _reflns_number_total 8215 _reflns_number_gt 6676 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ApexII (Bruker, 2004)' _computing_cell_refinement 'ApexII and SAINT (Bruker, 2001)' _computing_data_reduction SAINT _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 1999)' _computing_publication_material WinGX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+1.0224P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8215 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0783 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.46445(3) 0.78956(2) 0.798032(16) 0.01628(5) Uani 1 1 d . . . Co1 Co 0.18521(3) 0.33303(2) 0.782307(17) 0.01071(5) Uani 1 1 d . . . Cl3 Cl 0.68051(7) 0.95151(5) 0.90623(4) 0.02653(11) Uani 1 1 d . . . Cl2 Cl 0.19925(6) 0.81510(5) 0.78376(4) 0.02514(10) Uani 1 1 d . . . Cl1 Cl 0.51592(8) 0.75300(7) 0.64673(4) 0.03927(15) Uani 1 1 d . . . N3 N 0.35979(18) 0.28586(13) 0.73332(11) 0.0125(3) Uani 1 1 d . . . O3 O 0.47177(17) 0.64649(12) 0.87249(10) 0.0173(2) Uani 1 1 d . . . O1 O 0.36343(15) 0.44588(11) 0.89105(9) 0.0132(2) Uani 1 1 d . . . O2 O 0.25648(16) 0.49985(11) 0.75032(9) 0.0147(2) Uani 1 1 d . . . N2 N 0.01146(19) 0.21956(15) 0.66332(11) 0.0150(3) Uani 1 1 d . . . N4 N 0.01121(19) 0.36145(14) 0.84348(12) 0.0159(3) Uani 1 1 d . . . N1 N 0.16083(19) 0.18763(14) 0.84885(11) 0.0139(3) Uani 1 1 d . . . C10 C 0.4063(2) 0.19563(16) 0.77889(14) 0.0143(3) Uani 1 1 d . . . C4 C -0.0345(2) 0.09812(17) 0.67770(14) 0.0167(3) Uani 1 1 d . . . C18 C -0.2036(2) 0.4522(2) 0.87032(17) 0.0274(5) Uani 1 1 d . . . H18 H -0.2666 0.5068 0.8534 0.033 Uiso 1 1 calc R . . C3 C 0.1146(3) 0.22350(19) 0.94454(14) 0.0202(4) Uani 1 1 d . . . H3A H 0.0600 0.1484 0.9699 0.024 Uiso 1 1 calc R . . H3B H 0.2195 0.2747 0.9962 0.024 Uiso 1 1 calc R . . C15 C -0.0100(2) 0.29646(18) 0.92006(14) 0.0182(3) Uani 1 1 d . . . C12 C 0.5813(2) 0.1802(2) 0.66590(16) 0.0251(4) Uani 1 1 d . . . H12 H 0.6539 0.1427 0.6417 0.030 Uiso 1 1 calc R . . C2 C 0.3342(2) 0.16678(18) 0.86797(14) 0.0171(3) Uani 1 1 d . . . H2A H 0.3204 0.0800 0.8761 0.021 Uiso 1 1 calc R . . H2B H 0.4138 0.2216 0.9294 0.021 Uiso 1 1 calc R . . C17 C -0.2284(3) 0.3849(2) 0.94704(17) 0.0303(5) Uani 1 1 d . . . H17 H -0.3097 0.3929 0.9819 0.036 Uiso 1 1 calc R . . C8 C -0.0466(2) 0.2455(2) 0.56996(14) 0.0213(4) Uani 1 1 d . . . C20 C 0.3690(2) 0.53715(16) 0.83871(13) 0.0138(3) Uani 1 1 d . . . C14 C 0.4251(2) 0.32710(18) 0.65733(14) 0.0173(3) Uani 1 1 d . . . H14 H 0.3939 0.3910 0.6279 0.021 Uiso 1 1 calc R . . C19 C -0.0833(2) 0.43791(18) 0.81836(15) 0.0212(4) Uani 1 1 d . . . H19 H -0.0679 0.4819 0.7654 0.025 Uiso 1 1 calc R . . C11 C 0.5171(2) 0.13961(18) 0.74580(16) 0.0201(4) Uani 1 1 d . . . H11 H 0.5475 0.0763 0.7766 0.024 Uiso 1 1 calc R . . O4 O -0.1870(3) 0.6139(2) 0.6535(2) 0.0637(6) Uani 1 1 d . . . C7 C -0.1486(3) 0.1455(2) 0.49005(16) 0.0294(5) Uani 1 1 d . . . H7 H -0.1893 0.1629 0.4260 0.035 Uiso 1 1 calc R . . C5 C -0.1335(3) -0.0019(2) 0.60061(17) 0.0266(4) Uani 1 1 d . . . H5 H -0.1622 -0.0845 0.6128 0.032 Uiso 1 1 calc R . . C1 C 0.0178(2) 0.07596(17) 0.78344(15) 0.0186(3) Uani 1 1 d . . . H1A H 0.0571 0.0029 0.7834 0.022 Uiso 1 1 calc R . . H1B H -0.0831 0.0581 0.8110 0.022 Uiso 1 1 calc R . . C6 C -0.1885(3) 0.0241(2) 0.50521(18) 0.0322(5) Uani 1 1 d . . . H6 H -0.2529 -0.0414 0.4513 0.039 Uiso 1 1 calc R . . C16 C -0.1321(3) 0.3046(2) 0.97267(16) 0.0263(4) Uani 1 1 d . . . H16 H -0.1490 0.2575 1.0238 0.032 Uiso 1 1 calc R . . C9 C -0.0076(3) 0.3764(2) 0.55278(16) 0.0276(4) Uani 1 1 d . . . H9A H -0.0367 0.4250 0.6033 0.041 Uiso 1 1 calc R . . H9B H -0.0756 0.3784 0.4868 0.041 Uiso 1 1 calc R . . H9C H 0.1149 0.4116 0.5570 0.041 Uiso 1 1 calc R . . C13 C 0.5385(2) 0.2760(2) 0.62193(15) 0.0234(4) Uani 1 1 d . . . H13 H 0.5846 0.3055 0.5697 0.028 Uiso 1 1 calc R . . H101 H -0.296(8) 0.648(5) 0.648(4) 0.16(2) Uiso 1 1 d . . . H102 H -0.060(7) 0.687(5) 0.698(4) 0.133(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01621(10) 0.01602(11) 0.01823(11) 0.00742(8) 0.00587(8) 0.00531(8) Co1 0.01024(10) 0.01093(11) 0.01111(10) 0.00160(8) 0.00299(8) 0.00365(8) Cl3 0.0258(2) 0.0204(2) 0.0253(2) 0.00998(18) 0.00203(18) -0.00262(18) Cl2 0.0240(2) 0.0269(2) 0.0309(3) 0.0073(2) 0.00922(19) 0.0155(2) Cl1 0.0312(3) 0.0735(5) 0.0214(3) 0.0145(3) 0.0135(2) 0.0223(3) N3 0.0098(6) 0.0120(6) 0.0138(7) 0.0006(5) 0.0022(5) 0.0020(5) O3 0.0173(6) 0.0121(6) 0.0198(6) 0.0039(5) 0.0021(5) 0.0025(5) O1 0.0136(6) 0.0107(6) 0.0138(6) 0.0023(4) 0.0020(4) 0.0027(4) O2 0.0165(6) 0.0118(6) 0.0151(6) 0.0033(4) 0.0019(5) 0.0052(5) N2 0.0109(6) 0.0220(8) 0.0129(7) 0.0002(6) 0.0027(5) 0.0076(6) N4 0.0121(6) 0.0169(7) 0.0164(7) -0.0030(6) 0.0039(5) 0.0029(5) N1 0.0118(6) 0.0124(7) 0.0155(7) 0.0027(5) 0.0038(5) 0.0009(5) C10 0.0109(7) 0.0105(7) 0.0188(8) 0.0015(6) 0.0012(6) 0.0018(6) C4 0.0100(7) 0.0188(9) 0.0204(9) -0.0017(7) 0.0046(6) 0.0044(6) C18 0.0130(8) 0.0273(10) 0.0342(11) -0.0166(9) 0.0017(8) 0.0053(8) C3 0.0235(9) 0.0215(9) 0.0155(8) 0.0048(7) 0.0095(7) 0.0037(7) C15 0.0143(8) 0.0190(9) 0.0162(8) -0.0028(7) 0.0054(6) -0.0014(7) C12 0.0122(8) 0.0289(11) 0.0304(11) -0.0076(8) 0.0040(7) 0.0064(7) C2 0.0147(8) 0.0165(8) 0.0209(9) 0.0088(7) 0.0036(7) 0.0052(7) C17 0.0124(8) 0.0343(12) 0.0336(11) -0.0194(9) 0.0091(8) -0.0028(8) C8 0.0165(8) 0.0333(11) 0.0165(9) 0.0032(8) 0.0043(7) 0.0118(8) C20 0.0131(7) 0.0143(8) 0.0154(8) 0.0023(6) 0.0048(6) 0.0059(6) C14 0.0147(8) 0.0196(9) 0.0161(8) 0.0040(7) 0.0044(6) 0.0026(7) C19 0.0158(8) 0.0196(9) 0.0245(10) -0.0062(7) 0.0023(7) 0.0057(7) C11 0.0124(8) 0.0157(8) 0.0303(10) -0.0009(7) 0.0014(7) 0.0062(7) O4 0.0489(13) 0.0436(12) 0.0922(19) 0.0019(12) 0.0058(12) 0.0182(11) C7 0.0231(10) 0.0478(14) 0.0153(9) -0.0015(9) -0.0009(7) 0.0152(10) C5 0.0184(9) 0.0235(10) 0.0312(11) -0.0065(8) 0.0053(8) 0.0014(8) C1 0.0155(8) 0.0132(8) 0.0235(9) 0.0012(7) 0.0057(7) -0.0003(6) C6 0.0250(11) 0.0339(12) 0.0267(11) -0.0100(9) 0.0002(8) 0.0031(9) C16 0.0192(9) 0.0284(10) 0.0219(10) -0.0089(8) 0.0102(8) -0.0059(8) C9 0.0286(11) 0.0316(11) 0.0220(10) 0.0082(8) 0.0025(8) 0.0109(9) C13 0.0146(8) 0.0342(11) 0.0190(9) 0.0002(8) 0.0076(7) 0.0035(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.9954(13) . ? Zn1 Cl1 2.2423(6) . ? Zn1 Cl3 2.2597(6) . ? Zn1 Cl2 2.2654(6) . ? Co1 O1 1.8896(12) . ? Co1 N3 1.9116(14) . ? Co1 N4 1.9126(14) . ? Co1 O2 1.9195(12) . ? Co1 N1 1.9296(15) . ? Co1 N2 1.9601(15) . ? Co1 C20 2.2954(18) . ? N3 C14 1.341(2) . ? N3 C10 1.346(2) . ? O3 C20 1.246(2) . ? O1 C20 1.304(2) . ? O2 C20 1.298(2) . ? N2 C4 1.353(2) . ? N2 C8 1.356(2) . ? N4 C19 1.343(2) . ? N4 C15 1.351(2) . ? N1 C1 1.491(2) . ? N1 C2 1.491(2) . ? N1 C3 1.504(2) . ? C10 C11 1.387(2) . ? C10 C2 1.501(2) . ? C4 C5 1.380(3) . ? C4 C1 1.487(3) . ? C18 C17 1.373(3) . ? C18 C19 1.387(3) . ? C18 H18 0.9300 . ? C3 C15 1.499(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C15 C16 1.389(2) . ? C12 C13 1.379(3) . ? C12 C11 1.383(3) . ? C12 H12 0.9300 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C17 C16 1.391(3) . ? C17 H17 0.9300 . ? C8 C7 1.406(3) . ? C8 C9 1.466(3) . ? C14 C13 1.387(3) . ? C14 H14 0.9300 . ? C19 H19 0.9300 . ? C11 H11 0.9300 . ? O4 H101 1.07(6) . ? O4 H102 1.13(6) . ? C7 C6 1.357(3) . ? C7 H7 0.9300 . ? C5 C6 1.376(3) . ? C5 H5 0.9300 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C6 H6 0.9300 . ? C16 H16 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C13 H13 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 Cl1 110.59(4) . . ? O3 Zn1 Cl3 101.15(4) . . ? Cl1 Zn1 Cl3 113.13(2) . . ? O3 Zn1 Cl2 107.93(4) . . ? Cl1 Zn1 Cl2 112.17(2) . . ? Cl3 Zn1 Cl2 111.23(2) . . ? O1 Co1 N3 89.55(6) . . ? O1 Co1 N4 89.95(6) . . ? N3 Co1 N4 171.54(6) . . ? O1 Co1 O2 69.03(5) . . ? N3 Co1 O2 93.56(6) . . ? N4 Co1 O2 94.15(6) . . ? O1 Co1 N1 95.33(6) . . ? N3 Co1 N1 86.26(6) . . ? N4 Co1 N1 85.38(6) . . ? O2 Co1 N1 164.35(6) . . ? O1 Co1 N2 175.93(6) . . ? N3 Co1 N2 87.29(6) . . ? N4 Co1 N2 93.55(6) . . ? O2 Co1 N2 108.61(6) . . ? N1 Co1 N2 87.03(6) . . ? O1 Co1 C20 34.61(6) . . ? N3 Co1 C20 91.64(6) . . ? N4 Co1 C20 92.73(6) . . ? O2 Co1 C20 34.42(6) . . ? N1 Co1 C20 129.94(6) . . ? N2 Co1 C20 142.90(6) . . ? C14 N3 C10 120.62(15) . . ? C14 N3 Co1 126.60(12) . . ? C10 N3 Co1 112.61(11) . . ? C20 O3 Zn1 122.17(12) . . ? C20 O1 Co1 89.98(10) . . ? C20 O2 Co1 88.86(10) . . ? C4 N2 C8 118.98(16) . . ? C4 N2 Co1 111.84(12) . . ? C8 N2 Co1 128.62(14) . . ? C19 N4 C15 120.30(16) . . ? C19 N4 Co1 126.62(13) . . ? C15 N4 Co1 113.07(12) . . ? C1 N1 C2 111.58(14) . . ? C1 N1 C3 110.27(14) . . ? C2 N1 C3 113.16(14) . . ? C1 N1 Co1 110.36(11) . . ? C2 N1 Co1 105.91(10) . . ? C3 N1 Co1 105.26(11) . . ? N3 C10 C11 120.90(17) . . ? N3 C10 C2 114.47(15) . . ? C11 C10 C2 124.59(16) . . ? N2 C4 C5 122.99(18) . . ? N2 C4 C1 116.74(16) . . ? C5 C4 C1 120.17(18) . . ? C17 C18 C19 119.2(2) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C15 C3 N1 107.83(15) . . ? C15 C3 H3A 110.1 . . ? N1 C3 H3A 110.1 . . ? C15 C3 H3B 110.1 . . ? N1 C3 H3B 110.1 . . ? H3A C3 H3B 108.5 . . ? N4 C15 C16 121.08(19) . . ? N4 C15 C3 114.06(15) . . ? C16 C15 C3 124.78(18) . . ? C13 C12 C11 120.48(17) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? N1 C2 C10 107.97(14) . . ? N1 C2 H2A 110.1 . . ? C10 C2 H2A 110.1 . . ? N1 C2 H2B 110.1 . . ? C10 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? C18 C17 C16 120.04(18) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? N2 C8 C7 119.27(19) . . ? N2 C8 C9 120.53(18) . . ? C7 C8 C9 120.18(19) . . ? O3 C20 O2 125.64(16) . . ? O3 C20 O1 122.23(16) . . ? O2 C20 O1 112.13(15) . . ? O3 C20 Co1 177.62(14) . . ? O2 C20 Co1 56.73(8) . . ? O1 C20 Co1 55.41(8) . . ? N3 C14 C13 121.06(17) . . ? N3 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? N4 C19 C18 121.0(2) . . ? N4 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C12 C11 C10 118.39(18) . . ? C12 C11 H11 120.8 . . ? C10 C11 H11 120.8 . . ? H101 O4 H102 112(4) . . ? C6 C7 C8 120.9(2) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C6 C5 C4 118.1(2) . . ? C6 C5 H5 121.0 . . ? C4 C5 H5 121.0 . . ? C4 C1 N1 111.37(15) . . ? C4 C1 H1A 109.4 . . ? N1 C1 H1A 109.4 . . ? C4 C1 H1B 109.4 . . ? N1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C7 C6 C5 119.8(2) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C15 C16 C17 118.4(2) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C13 C14 118.48(18) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.859 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.091 #===END data_lma3 _database_code_depnum_ccdc_archive 'CCDC 686137' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H20 Cl3 Co N4 O3 Zn' _chemical_formula_weight 595.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2916(7) _cell_length_b 11.0966(11) _cell_length_c 14.0994(13) _cell_angle_alpha 95.851(4) _cell_angle_beta 102.607(4) _cell_angle_gamma 108.600(4) _cell_volume 1179.04(19) _cell_formula_units_Z 2 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 7611 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 34.38 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 2.090 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.769623 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SQUEEZE _exptl_special_details ; ? ; _diffrn_ambient_temperature 85(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa ApexII area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 20348 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 34.74 _reflns_number_total 9494 _reflns_number_gt 7372 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ApexII (Bruker, 2004)' _computing_cell_refinement 'ApexII and SAINT (Bruker, 2001)' _computing_data_reduction SAINT _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 1999)' _computing_publication_material WinGX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.0235P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9494 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0815 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.02176(2) -0.295998(18) 0.190646(13) 0.01414(5) Uani 1 1 d . . . Co1 Co 0.32102(2) 0.173196(19) 0.218723(14) 0.00934(5) Uani 1 1 d . . . Cl1 Cl -0.06493(6) -0.28812(5) 0.33233(3) 0.02773(10) Uani 1 1 d . . . Cl2 Cl 0.29889(5) -0.30144(4) 0.21682(3) 0.02084(8) Uani 1 1 d . . . Cl3 Cl -0.17735(5) -0.46367(4) 0.07616(3) 0.02084(8) Uani 1 1 d . . . O1 O 0.13625(13) 0.05935(10) 0.11051(8) 0.0120(2) Uani 1 1 d . . . O2 O 0.23656(14) 0.00243(10) 0.24721(8) 0.0130(2) Uani 1 1 d . . . O3 O 0.01421(14) -0.14596(11) 0.12606(8) 0.0167(2) Uani 1 1 d . . . N2 N 0.15190(16) 0.22479(13) 0.26783(9) 0.0118(2) Uani 1 1 d . . . N3 N 0.49233(16) 0.13943(13) 0.15777(9) 0.0121(2) Uani 1 1 d . . . C10 C 0.10244(19) 0.31243(15) 0.22073(11) 0.0133(3) Uani 1 1 d . . . N1 N 0.35287(17) 0.32082(13) 0.15276(10) 0.0143(2) Uani 1 1 d . . . C6 C 0.6612(2) 0.43923(17) 0.47536(12) 0.0194(3) Uani 1 1 d . . . H6 H 0.7045 0.5282 0.4981 0.023 Uiso 1 1 calc R . . C8 C 0.6400(2) 0.22709(19) 0.50162(12) 0.0215(3) Uani 1 1 d . . . H8 H 0.6672 0.1709 0.5417 0.026 Uiso 1 1 calc R . . N4 N 0.49133(16) 0.25891(13) 0.34543(9) 0.0128(2) Uani 1 1 d . . . C3 C 0.17927(19) 0.34271(16) 0.13492(12) 0.0156(3) Uani 1 1 d . . . H3A H 0.1973 0.4320 0.1285 0.019 Uiso 1 1 calc R . . H3B H 0.0986 0.2873 0.0741 0.019 Uiso 1 1 calc R . . C4 C 0.3929(2) 0.27744(17) 0.05784(11) 0.0173(3) Uani 1 1 d . . . H4A H 0.2846 0.2232 0.0092 0.021 Uiso 1 1 calc R . . H4B H 0.4488 0.3520 0.0308 0.021 Uiso 1 1 calc R . . C16 C 0.6353(2) 0.19142(18) 0.03019(12) 0.0203(3) Uani 1 1 d . . . H16 H 0.6523 0.2368 -0.0209 0.024 Uiso 1 1 calc R . . C5 C 0.55213(18) 0.38779(15) 0.37942(11) 0.0141(3) Uani 1 1 d . . . C15 C 0.5152(2) 0.20240(15) 0.08196(11) 0.0147(3) Uani 1 1 d . . . C18 C 0.7043(2) 0.04542(17) 0.13287(13) 0.0212(3) Uani 1 1 d . . . H18 H 0.7667 -0.0088 0.1505 0.025 Uiso 1 1 calc R . . C11 C -0.0086(2) 0.36892(17) 0.25224(13) 0.0193(3) Uani 1 1 d . . . H11 H -0.0440 0.4282 0.2190 0.023 Uiso 1 1 calc R . . C19 C 0.5841(2) 0.06171(16) 0.18305(12) 0.0165(3) Uani 1 1 d . . . H19 H 0.5665 0.0182 0.2350 0.020 Uiso 1 1 calc R . . C12 C -0.0653(2) 0.33467(19) 0.33454(13) 0.0227(4) Uani 1 1 d . . . H12 H -0.1375 0.3726 0.3581 0.027 Uiso 1 1 calc R . . C20 C 0.12395(19) -0.03383(15) 0.16001(11) 0.0121(3) Uani 1 1 d . . . C2 C 0.5029(2) 0.47586(16) 0.31401(12) 0.0164(3) Uani 1 1 d . . . H2A H 0.5854 0.5634 0.3403 0.020 Uiso 1 1 calc R . . H2B H 0.3864 0.4752 0.3160 0.020 Uiso 1 1 calc R . . C17 C 0.7298(2) 0.11120(18) 0.05622(13) 0.0233(4) Uani 1 1 d . . . H17 H 0.8103 0.1017 0.0220 0.028 Uiso 1 1 calc R . . C9 C 0.5343(2) 0.18020(17) 0.40617(12) 0.0171(3) Uani 1 1 d . . . H9 H 0.4909 0.0914 0.3826 0.021 Uiso 1 1 calc R . . C14 C 0.0938(2) 0.18929(17) 0.34595(11) 0.0165(3) Uani 1 1 d . . . H14 H 0.1266 0.1271 0.3765 0.020 Uiso 1 1 calc R . . C7 C 0.7047(2) 0.35844(19) 0.53648(12) 0.0223(4) Uani 1 1 d . . . H7 H 0.7769 0.3924 0.6004 0.027 Uiso 1 1 calc R . . C1 C 0.5020(2) 0.44015(16) 0.20775(11) 0.0158(3) Uani 1 1 d . . . H1A H 0.4960 0.5114 0.1743 0.019 Uiso 1 1 calc R . . H1B H 0.6122 0.4279 0.2062 0.019 Uiso 1 1 calc R . . C13 C -0.0143(2) 0.24410(19) 0.38141(13) 0.0221(4) Uani 1 1 d . . . H13 H -0.0525 0.2203 0.4363 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01539(8) 0.01321(9) 0.01256(9) 0.00335(6) 0.00261(6) 0.00379(7) Co1 0.00974(8) 0.00973(9) 0.00820(9) 0.00118(7) 0.00218(6) 0.00324(7) Cl1 0.01956(18) 0.0461(3) 0.01547(18) 0.00464(18) 0.00615(14) 0.00809(19) Cl2 0.02096(18) 0.0232(2) 0.0237(2) 0.00738(15) 0.00786(14) 0.01269(16) Cl3 0.02537(19) 0.01456(18) 0.01554(18) 0.00272(14) 0.00276(14) -0.00056(14) O1 0.0126(4) 0.0114(5) 0.0104(5) 0.0014(4) 0.0007(4) 0.0040(4) O2 0.0136(5) 0.0119(5) 0.0115(5) 0.0029(4) 0.0001(4) 0.0040(4) O3 0.0157(5) 0.0117(5) 0.0175(5) 0.0024(4) -0.0021(4) 0.0026(4) N2 0.0107(5) 0.0125(6) 0.0108(5) 0.0000(4) 0.0032(4) 0.0027(4) N3 0.0111(5) 0.0126(6) 0.0111(6) -0.0013(4) 0.0020(4) 0.0038(4) C10 0.0109(6) 0.0120(7) 0.0143(7) 0.0002(5) 0.0011(5) 0.0025(5) N1 0.0152(6) 0.0147(6) 0.0139(6) 0.0035(5) 0.0054(5) 0.0051(5) C6 0.0137(6) 0.0229(8) 0.0168(7) -0.0059(6) 0.0021(5) 0.0043(6) C8 0.0188(7) 0.0321(10) 0.0138(7) 0.0065(7) 0.0023(6) 0.0099(7) N4 0.0103(5) 0.0162(6) 0.0112(6) 0.0006(5) 0.0033(4) 0.0041(5) C3 0.0147(6) 0.0158(7) 0.0177(7) 0.0074(6) 0.0040(5) 0.0062(6) C4 0.0207(7) 0.0188(8) 0.0107(7) 0.0020(6) 0.0042(5) 0.0048(6) C16 0.0170(7) 0.0215(8) 0.0149(7) -0.0056(6) 0.0063(6) -0.0018(6) C5 0.0096(6) 0.0176(7) 0.0141(7) 0.0002(5) 0.0032(5) 0.0043(5) C15 0.0141(6) 0.0140(7) 0.0115(6) -0.0024(5) 0.0033(5) 0.0005(5) C18 0.0129(6) 0.0203(8) 0.0250(8) -0.0088(6) 0.0001(6) 0.0061(6) C11 0.0134(7) 0.0176(8) 0.0241(8) -0.0012(6) 0.0022(6) 0.0054(6) C19 0.0141(6) 0.0159(7) 0.0170(7) -0.0021(6) 0.0003(5) 0.0060(6) C12 0.0131(7) 0.0285(9) 0.0240(8) -0.0064(7) 0.0056(6) 0.0070(7) C20 0.0128(6) 0.0124(7) 0.0115(6) 0.0011(5) 0.0020(5) 0.0060(5) C2 0.0151(6) 0.0155(7) 0.0176(7) 0.0005(6) 0.0048(5) 0.0044(6) C17 0.0136(7) 0.0243(9) 0.0240(9) -0.0124(7) 0.0067(6) -0.0003(6) C9 0.0158(7) 0.0202(8) 0.0146(7) 0.0045(6) 0.0030(5) 0.0057(6) C14 0.0142(6) 0.0225(8) 0.0117(7) 0.0035(6) 0.0045(5) 0.0040(6) C7 0.0179(7) 0.0337(10) 0.0119(7) -0.0032(6) 0.0006(5) 0.0089(7) C1 0.0156(6) 0.0138(7) 0.0158(7) 0.0014(5) 0.0038(5) 0.0027(6) C13 0.0155(7) 0.0333(10) 0.0158(7) 0.0006(7) 0.0070(6) 0.0056(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. The structure was found to contain sigificant electron density which could not be reasonably assigned and was thought to indicate the presence of one or more disordered solvent molecules. The SQUEEZE option within PLATON generated a modified hkl file, which when used in subsequent least squares cycles, gave significantly improved R factors and, most importantly, a stable refinement. SQUEEZE gave an electron count of 24 per cell in a total void volume of 100.4 \%A^3^. Given that Z = 2, this corresponds to 2.4 disordered water molecules per cell, or 1.2 water molecules per cation. The details of the SQUEEZE procedure are included at the end of this file. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.9889(12) . ? Zn1 Cl3 2.2490(5) . ? Zn1 Cl2 2.2678(5) . ? Zn1 Cl1 2.2686(5) . ? Co1 O1 1.9034(10) . ? Co1 N2 1.9049(13) . ? Co1 O2 1.9167(11) . ? Co1 N3 1.9244(13) . ? Co1 N1 1.9391(14) . ? Co1 N4 1.9458(12) . ? Co1 C20 2.2934(15) . ? O1 C20 1.2951(19) . ? O2 C20 1.3052(17) . ? O3 C20 1.2536(18) . ? N2 C14 1.342(2) . ? N2 C10 1.350(2) . ? N3 C19 1.346(2) . ? N3 C15 1.350(2) . ? C10 C11 1.388(2) . ? C10 C3 1.505(2) . ? N1 C1 1.487(2) . ? N1 C3 1.5072(19) . ? N1 C4 1.516(2) . ? C6 C7 1.380(3) . ? C6 C5 1.397(2) . ? C6 H6 0.9300 . ? C8 C7 1.376(3) . ? C8 C9 1.379(2) . ? C8 H8 0.9300 . ? N4 C5 1.351(2) . ? N4 C9 1.357(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C15 1.511(2) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C16 C15 1.385(2) . ? C16 C17 1.388(3) . ? C16 H16 0.9300 . ? C5 C2 1.499(2) . ? C18 C17 1.381(3) . ? C18 C19 1.387(2) . ? C18 H18 0.9300 . ? C11 C12 1.388(3) . ? C11 H11 0.9300 . ? C19 H19 0.9300 . ? C12 C13 1.382(3) . ? C12 H12 0.9300 . ? C2 C1 1.508(2) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C17 H17 0.9300 . ? C9 H9 0.9300 . ? C14 C13 1.380(2) . ? C14 H14 0.9300 . ? C7 H7 0.9300 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C13 H13 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 Cl3 102.05(3) . . ? O3 Zn1 Cl2 108.20(4) . . ? Cl3 Zn1 Cl2 112.388(18) . . ? O3 Zn1 Cl1 112.02(4) . . ? Cl3 Zn1 Cl1 109.716(19) . . ? Cl2 Zn1 Cl1 112.066(17) . . ? O1 Co1 N2 89.59(5) . . ? O1 Co1 O2 69.06(5) . . ? N2 Co1 O2 93.22(5) . . ? O1 Co1 N3 89.78(5) . . ? N2 Co1 N3 171.92(6) . . ? O2 Co1 N3 94.07(5) . . ? O1 Co1 N1 93.67(5) . . ? N2 Co1 N1 86.55(6) . . ? O2 Co1 N1 162.73(5) . . ? N3 Co1 N1 85.45(6) . . ? O1 Co1 N4 167.19(5) . . ? N2 Co1 N4 87.98(5) . . ? O2 Co1 N4 98.52(5) . . ? N3 Co1 N4 94.37(5) . . ? N1 Co1 N4 98.73(6) . . ? O1 Co1 C20 34.38(5) . . ? N2 Co1 C20 91.60(5) . . ? O2 Co1 C20 34.68(5) . . ? N3 Co1 C20 92.42(5) . . ? N1 Co1 C20 128.05(5) . . ? N4 Co1 C20 133.12(6) . . ? C20 O1 Co1 89.53(8) . . ? C20 O2 Co1 88.65(9) . . ? C20 O3 Zn1 122.57(10) . . ? C14 N2 C10 120.75(13) . . ? C14 N2 Co1 125.90(11) . . ? C10 N2 Co1 113.14(10) . . ? C19 N3 C15 120.18(14) . . ? C19 N3 Co1 126.73(11) . . ? C15 N3 Co1 113.09(10) . . ? N2 C10 C11 120.96(15) . . ? N2 C10 C3 114.49(13) . . ? C11 C10 C3 124.55(15) . . ? C1 N1 C3 111.33(12) . . ? C1 N1 C4 107.85(12) . . ? C3 N1 C4 112.83(12) . . ? C1 N1 Co1 115.02(10) . . ? C3 N1 Co1 105.29(9) . . ? C4 N1 Co1 104.44(10) . . ? C7 C6 C5 120.20(16) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C7 C8 C9 118.85(16) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C5 N4 C9 119.23(13) . . ? C5 N4 Co1 124.27(11) . . ? C9 N4 Co1 116.09(11) . . ? C10 C3 N1 108.84(12) . . ? C10 C3 H3A 109.9 . . ? N1 C3 H3A 109.9 . . ? C10 C3 H3B 109.9 . . ? N1 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? C15 C4 N1 107.81(12) . . ? C15 C4 H4A 110.1 . . ? N1 C4 H4A 110.1 . . ? C15 C4 H4B 110.1 . . ? N1 C4 H4B 110.1 . . ? H4A C4 H4B 108.5 . . ? C15 C16 C17 118.52(17) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? N4 C5 C6 120.14(15) . . ? N4 C5 C2 119.93(13) . . ? C6 C5 C2 119.92(15) . . ? N3 C15 C16 121.27(15) . . ? N3 C15 C4 113.76(13) . . ? C16 C15 C4 124.90(15) . . ? C17 C18 C19 118.83(16) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C12 C11 C10 118.35(16) . . ? C12 C11 H11 120.8 . . ? C10 C11 H11 120.8 . . ? N3 C19 C18 121.10(16) . . ? N3 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C13 C12 C11 119.87(15) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? O3 C20 O1 122.43(13) . . ? O3 C20 O2 124.81(14) . . ? O1 C20 O2 112.76(13) . . ? O3 C20 Co1 178.50(12) . . ? O1 C20 Co1 56.09(7) . . ? O2 C20 Co1 56.67(7) . . ? C5 C2 C1 114.16(13) . . ? C5 C2 H2A 108.7 . . ? C1 C2 H2A 108.7 . . ? C5 C2 H2B 108.7 . . ? C1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C18 C17 C16 120.08(16) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? N4 C9 C8 122.36(16) . . ? N4 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? N2 C14 C13 120.66(16) . . ? N2 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C8 C7 C6 119.21(15) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? N1 C1 C2 113.57(13) . . ? N1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? N1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C14 C13 C12 119.38(16) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.160 _refine_diff_density_min -0.871 _refine_diff_density_rms 0.101 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.500 99.4 24.3 _platon_squeeze_details ; ? ; #===END data_lmc3 _database_code_depnum_ccdc_archive 'CCDC 686138' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H54 Cl8 Co2 N14 O13 Zn3' _chemical_formula_weight 1440.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.9731(9) _cell_length_b 17.371(5) _cell_length_c 15.764(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.376(5) _cell_angle_gamma 90.00 _cell_volume 5348(2) _cell_formula_units_Z 4 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 9294 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 29.60 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.789 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912 _exptl_absorpt_coefficient_mu 2.403 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.731833 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 85(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa ApexII area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 118100 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 29.74 _reflns_number_total 15187 _reflns_number_gt 12734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ApexII (Bruker, 2004)' _computing_cell_refinement 'ApexII and SAINT (Bruker, 2001)' _computing_data_reduction SAINT _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 1999)' _computing_publication_material WinGX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+3.5040P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15187 _refine_ls_number_parameters 697 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0548 _refine_ls_wR_factor_gt 0.0515 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.253718(9) -0.296985(10) 0.842621(12) 0.01194(4) Uani 1 1 d . . . Zn2 Zn 0.244117(10) 0.337390(11) 0.648496(13) 0.01515(4) Uani 1 1 d . . . Zn3 Zn 0.272752(9) 0.012047(10) 0.705669(12) 0.01055(4) Uani 1 1 d . . . Co1 Co 0.026436(11) -0.002446(12) 0.721761(14) 0.01162(4) Uani 1 1 d . . . Co2 Co 0.518505(10) 0.135579(11) 0.819267(14) 0.00867(4) Uani 1 1 d . . . Cl1 Cl 0.19470(2) -0.21973(2) 0.90472(3) 0.01640(8) Uani 1 1 d . . . Cl2 Cl 0.34718(2) -0.23272(2) 0.84219(3) 0.01501(7) Uani 1 1 d . . . Cl3 Cl 0.190570(19) -0.33584(2) 0.69862(3) 0.01520(7) Uani 1 1 d . . . Cl4 Cl 0.28444(2) -0.40575(2) 0.92901(3) 0.01706(8) Uani 1 1 d . . . Cl5 Cl 0.31180(2) 0.35643(3) 0.79635(3) 0.02785(10) Uani 1 1 d . . . Cl6 Cl 0.31332(2) 0.27153(2) 0.58788(3) 0.01740(8) Uani 1 1 d . . . Cl7 Cl 0.20369(2) 0.44585(2) 0.56920(3) 0.02005(8) Uani 1 1 d . . . Cl8 Cl 0.15698(2) 0.25484(2) 0.63426(3) 0.02410(9) Uani 1 1 d . . . O1 O 0.26398(7) -0.00462(9) 0.83264(9) 0.0235(3) Uani 1 1 d . . . O2 O 0.27591(7) 0.13250(7) 0.71924(10) 0.0208(3) Uani 1 1 d . . . O3 O 0.27535(7) -0.10555(7) 0.68635(9) 0.0187(2) Uani 1 1 d . . . O4 O 0.27831(7) 0.02227(8) 0.57700(9) 0.0208(3) Uani 1 1 d . . . O5 O 0.24645(7) 0.13723(8) 0.45024(10) 0.0228(3) Uani 1 1 d . . . O6 O 0.17314(7) -0.31233(8) 1.06638(10) 0.0231(3) Uani 1 1 d . . . O11 O 0.05451(5) 0.02764(6) 0.62491(7) 0.0132(2) Uani 1 1 d . . . O12 O 0.12284(5) -0.01791(6) 0.75325(7) 0.0135(2) Uani 1 1 d . . . O13 O 0.16605(5) 0.01795(6) 0.64649(7) 0.0142(2) Uani 1 1 d . . . O21 O 0.48980(5) 0.03207(6) 0.81582(7) 0.0112(2) Uani 1 1 d . . . O22 O 0.42006(5) 0.12749(6) 0.76714(7) 0.0111(2) Uani 1 1 d . . . O23 O 0.37772(5) 0.00700(6) 0.76821(8) 0.0135(2) Uani 1 1 d . . . N1 N -0.07306(7) 0.02310(8) 0.66040(9) 0.0131(3) Uani 1 1 d . . . N2 N 0.61958(6) 0.11578(7) 0.87770(8) 0.0104(2) Uani 1 1 d . . . N11 N 0.02254(7) -0.04058(8) 0.83495(9) 0.0152(3) Uani 1 1 d . . . N12 N 0.01284(7) -0.10636(8) 0.67248(9) 0.0139(3) Uani 1 1 d . . . N13 N 0.04865(7) 0.09951(8) 0.77235(9) 0.0161(3) Uani 1 1 d . . . N14 N -0.03402(7) -0.04457(8) 0.85699(9) 0.0153(3) Uani 1 1 d . . . N15 N -0.03382(7) -0.12841(8) 0.59066(9) 0.0143(3) Uani 1 1 d . . . N16 N 0.02593(7) 0.16337(8) 0.72083(10) 0.0170(3) Uani 1 1 d . . . N21 N 0.52378(7) 0.24605(7) 0.81213(9) 0.0111(2) Uani 1 1 d . . . N22 N 0.50827(7) 0.14746(7) 0.93424(9) 0.0112(2) Uani 1 1 d . . . N23 N 0.51895(7) 0.12293(7) 0.69676(9) 0.0121(3) Uani 1 1 d . . . N24 N 0.58007(7) 0.29034(7) 0.85048(9) 0.0125(3) Uani 1 1 d . . . N25 N 0.53955(7) 0.10143(7) 1.00676(9) 0.0117(2) Uani 1 1 d . . . N26 N 0.56438(7) 0.08279(8) 0.67082(9) 0.0144(3) Uani 1 1 d . . . C1 C -0.11776(8) -0.01451(10) 0.70467(11) 0.0161(3) Uani 1 1 d . . . H1A H -0.1184 -0.0696 0.6942 0.019 Uiso 1 1 calc R . . H1B H -0.1642 0.0044 0.6755 0.019 Uiso 1 1 calc R . . C2 C -0.09495(9) -0.00023(10) 0.80607(11) 0.0182(3) Uani 1 1 d . . . H2A H -0.0854 0.0542 0.8181 0.022 Uiso 1 1 calc R . . H2B H -0.1317 -0.0140 0.8267 0.022 Uiso 1 1 calc R . . C3 C -0.09527(8) -0.00299(9) 0.56257(11) 0.0147(3) Uani 1 1 d . . . H3A H -0.1402 0.0185 0.5293 0.018 Uiso 1 1 calc R . . H3B H -0.0638 0.0185 0.5365 0.018 Uiso 1 1 calc R . . C4 C -0.09876(8) -0.08876(9) 0.54735(11) 0.0155(3) Uani 1 1 d . . . H4A H -0.1320 -0.1102 0.5703 0.019 Uiso 1 1 calc R . . H4B H -0.1150 -0.0986 0.4823 0.019 Uiso 1 1 calc R . . C5 C -0.08768(8) 0.10854(9) 0.65691(11) 0.0160(3) Uani 1 1 d . . . H5A H -0.0906 0.1240 0.7145 0.019 Uiso 1 1 calc R . . H5B H -0.1320 0.1180 0.6097 0.019 Uiso 1 1 calc R . . C6 C -0.03486(8) 0.15845(9) 0.63861(11) 0.0173(3) Uani 1 1 d . . . H6A H -0.0232 0.1364 0.5896 0.021 Uiso 1 1 calc R . . H6B H -0.0534 0.2095 0.6202 0.021 Uiso 1 1 calc R . . C7 C 0.66069(8) 0.18348(9) 0.86836(11) 0.0143(3) Uani 1 1 d . . . H7A H 0.6521 0.1916 0.8043 0.017 Uiso 1 1 calc R . . H7B H 0.7089 0.1717 0.8984 0.017 Uiso 1 1 calc R . . C8 C 0.64506(8) 0.25705(9) 0.90790(11) 0.0151(3) Uani 1 1 d . . . H8A H 0.6438 0.2465 0.9677 0.018 Uiso 1 1 calc R . . H8B H 0.6814 0.2939 0.9152 0.018 Uiso 1 1 calc R . . C9 C 0.64464(8) 0.09489(9) 0.97774(11) 0.0148(3) Uani 1 1 d . . . H9A H 0.6862 0.0647 0.9923 0.018 Uiso 1 1 calc R . . H9B H 0.6564 0.1419 1.0132 0.018 Uiso 1 1 calc R . . C10 C 0.59446(8) 0.05039(9) 1.00668(11) 0.0138(3) Uani 1 1 d . . . H10A H 0.5758 0.0080 0.9650 0.017 Uiso 1 1 calc R . . H10B H 0.6175 0.0293 1.0672 0.017 Uiso 1 1 calc R . . C11 C 0.63591(8) 0.04735(9) 0.83078(11) 0.0156(3) Uani 1 1 d . . . H11A H 0.6049 0.0059 0.8309 0.019 Uiso 1 1 calc R . . H11B H 0.6819 0.0303 0.8665 0.019 Uiso 1 1 calc R . . C12 C 0.63146(8) 0.05960(10) 0.73424(11) 0.0172(3) Uani 1 1 d . . . H12A H 0.6645 0.0987 0.7342 0.021 Uiso 1 1 calc R . . H12B H 0.6445 0.0122 0.7124 0.021 Uiso 1 1 calc R . . C13 C 0.11811(8) 0.00953(9) 0.67343(10) 0.0124(3) Uani 1 1 d . . . C14 C 0.42569(8) 0.05330(8) 0.78198(10) 0.0108(3) Uani 1 1 d . . . C15 C -0.02067(9) -0.08363(10) 0.93536(11) 0.0187(3) Uani 1 1 d . . . H15 H -0.0514 -0.0934 0.9642 0.022 Uiso 1 1 calc R . . C16 C 0.04675(9) -0.10649(10) 0.96495(12) 0.0203(3) Uani 1 1 d . . . H16 H 0.0706 -0.1347 1.0170 0.024 Uiso 1 1 calc R . . C17 C 0.07166(9) -0.07849(10) 0.90063(11) 0.0177(3) Uani 1 1 d . . . H17 H 0.1162 -0.0851 0.9029 0.021 Uiso 1 1 calc R . . C18 C -0.01798(9) -0.19813(10) 0.56690(12) 0.0186(3) Uani 1 1 d . . . H18 H -0.0429 -0.2253 0.5144 0.022 Uiso 1 1 calc R . . C19 C 0.04153(9) -0.22200(10) 0.63397(12) 0.0197(3) Uani 1 1 d . . . H19 H 0.0650 -0.2678 0.6360 0.024 Uiso 1 1 calc R . . C20 C 0.05932(8) -0.16334(9) 0.69796(12) 0.0171(3) Uani 1 1 d . . . H20 H 0.0980 -0.1634 0.7511 0.020 Uiso 1 1 calc R . . C21 C 0.06351(9) 0.22477(10) 0.76092(14) 0.0247(4) Uani 1 1 d . . . H21 H 0.0573 0.2749 0.7386 0.030 Uiso 1 1 calc R . . C22 C 0.11286(10) 0.20040(11) 0.84098(14) 0.0276(4) Uani 1 1 d . . . H22 H 0.1464 0.2302 0.8832 0.033 Uiso 1 1 calc R . . C23 C 0.10204(9) 0.12188(11) 0.84550(12) 0.0220(4) Uani 1 1 d . . . H23 H 0.1280 0.0896 0.8924 0.026 Uiso 1 1 calc R . . C24 C 0.56362(9) 0.36546(9) 0.83699(11) 0.0168(3) Uani 1 1 d . . . H24 H 0.5937 0.4067 0.8569 0.020 Uiso 1 1 calc R . . C25 C 0.49474(9) 0.37017(9) 0.78866(11) 0.0173(3) Uani 1 1 d . . . H25 H 0.4688 0.4146 0.7694 0.021 Uiso 1 1 calc R . . C26 C 0.47167(8) 0.29440(9) 0.77439(11) 0.0137(3) Uani 1 1 d . . . H26 H 0.4265 0.2796 0.7431 0.016 Uiso 1 1 calc R . . C27 C 0.51649(8) 0.11635(9) 1.07398(11) 0.0148(3) Uani 1 1 d . . . H27 H 0.5314 0.0931 1.1311 0.018 Uiso 1 1 calc R . . C28 C 0.46691(9) 0.17198(9) 1.04346(11) 0.0172(3) Uani 1 1 d . . . H28 H 0.4412 0.1932 1.0748 0.021 Uiso 1 1 calc R . . C29 C 0.46322(8) 0.19004(9) 0.95597(11) 0.0153(3) Uani 1 1 d . . . H29 H 0.4338 0.2263 0.9181 0.018 Uiso 1 1 calc R . . C30 C 0.54211(9) 0.07713(10) 0.57965(11) 0.0195(3) Uani 1 1 d . . . H30 H 0.5650 0.0531 0.5463 0.023 Uiso 1 1 calc R . . C31 C 0.47969(9) 0.11307(10) 0.54432(12) 0.0203(3) Uani 1 1 d . . . H31 H 0.4518 0.1180 0.4833 0.024 Uiso 1 1 calc R . . C32 C 0.46715(9) 0.14046(9) 0.61964(11) 0.0167(3) Uani 1 1 d . . . H32 H 0.4281 0.1673 0.6168 0.020 Uiso 1 1 calc R . . O7 O 0.29220(13) 0.13344(15) 0.90892(15) 0.0891(8) Uani 1 1 d . . . H83 H 0.2628(13) 0.1349(15) 0.4135(18) 0.045(8) Uiso 1 1 d . . . H88 H 0.2432(14) 0.1599(15) 0.6901(18) 0.050(8) Uiso 1 1 d . . . H89 H 0.2390(13) -0.1305(15) 0.6494(18) 0.045(7) Uiso 1 1 d . . . H85 H 0.2710(12) 0.0570(14) 0.5411(16) 0.034(7) Uiso 1 1 d . . . H87 H 0.3095(15) 0.1504(15) 0.7182(18) 0.051(8) Uiso 1 1 d . . . H86 H 0.2808(12) -0.0142(14) 0.5493(16) 0.034(7) Uiso 1 1 d . . . H81 H 0.1803(13) -0.2962(15) 1.0276(18) 0.044(8) Uiso 1 1 d . . . H90 H 0.2931(13) -0.1309(14) 0.7286(17) 0.038(7) Uiso 1 1 d . . . H84 H 0.2624(13) 0.1751(15) 0.4805(17) 0.040(7) Uiso 1 1 d . . . H82 H 0.1699(14) -0.2764(16) 1.0972(19) 0.051(8) Uiso 1 1 d . . . H92 H 0.2242(14) -0.0160(15) 0.8205(18) 0.044(8) Uiso 1 1 d . . . H93 H 0.2716(13) 0.0337(16) 0.8609(18) 0.043(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01096(9) 0.01405(8) 0.01070(9) 0.00000(6) 0.00381(7) -0.00060(6) Zn2 0.01137(9) 0.01906(9) 0.01464(9) -0.00256(7) 0.00429(7) -0.00024(7) Zn3 0.00776(8) 0.01348(8) 0.00974(8) -0.00022(6) 0.00241(7) -0.00055(6) Co1 0.00726(10) 0.01854(10) 0.00874(10) 0.00190(8) 0.00253(8) 0.00192(8) Co2 0.00702(10) 0.00989(9) 0.00856(9) 0.00010(7) 0.00218(8) -0.00047(7) Cl1 0.01541(19) 0.01948(17) 0.01428(18) -0.00027(14) 0.00539(15) 0.00427(14) Cl2 0.01398(18) 0.01752(17) 0.01380(18) -0.00213(13) 0.00537(15) -0.00435(14) Cl3 0.01249(18) 0.02041(17) 0.01181(17) -0.00168(13) 0.00337(14) -0.00243(14) Cl4 0.0189(2) 0.01625(17) 0.01559(18) 0.00341(14) 0.00577(16) 0.00023(14) Cl5 0.0210(2) 0.0473(3) 0.0142(2) -0.00748(18) 0.00528(17) -0.00214(19) Cl6 0.01470(19) 0.02306(18) 0.01493(18) -0.00052(14) 0.00598(15) 0.00351(15) Cl7 0.0166(2) 0.01855(18) 0.0240(2) -0.00042(15) 0.00620(17) 0.00108(15) Cl8 0.0135(2) 0.0243(2) 0.0330(2) 0.00306(17) 0.00660(18) -0.00206(15) O1 0.0102(6) 0.0470(9) 0.0122(6) 0.0025(6) 0.0029(5) 0.0004(6) O2 0.0121(6) 0.0157(6) 0.0334(8) -0.0008(5) 0.0070(6) -0.0006(5) O3 0.0165(6) 0.0149(5) 0.0192(6) 0.0011(5) -0.0001(5) -0.0014(5) O4 0.0296(7) 0.0205(6) 0.0161(6) 0.0008(5) 0.0126(6) 0.0027(5) O5 0.0239(7) 0.0259(7) 0.0212(7) -0.0022(5) 0.0112(6) -0.0057(5) O6 0.0270(7) 0.0255(7) 0.0185(7) 0.0040(6) 0.0103(6) 0.0071(5) O11 0.0076(5) 0.0217(5) 0.0099(5) 0.0023(4) 0.0026(4) 0.0015(4) O12 0.0070(5) 0.0235(6) 0.0091(5) 0.0024(4) 0.0018(4) 0.0022(4) O13 0.0078(5) 0.0236(6) 0.0108(5) 0.0016(4) 0.0029(4) 0.0006(4) O21 0.0072(5) 0.0111(5) 0.0137(5) 0.0004(4) 0.0019(4) -0.0010(4) O22 0.0083(5) 0.0116(5) 0.0122(5) 0.0005(4) 0.0023(4) -0.0004(4) O23 0.0084(5) 0.0137(5) 0.0168(6) 0.0001(4) 0.0026(5) -0.0019(4) N1 0.0094(6) 0.0190(6) 0.0107(6) 0.0028(5) 0.0034(5) 0.0027(5) N2 0.0086(6) 0.0127(6) 0.0094(6) 0.0004(5) 0.0026(5) -0.0006(5) N11 0.0107(7) 0.0234(7) 0.0120(6) 0.0021(5) 0.0049(5) 0.0031(5) N12 0.0094(6) 0.0199(6) 0.0110(6) 0.0019(5) 0.0022(5) 0.0006(5) N13 0.0127(7) 0.0223(7) 0.0133(7) -0.0007(5) 0.0047(6) 0.0015(5) N14 0.0124(7) 0.0228(7) 0.0120(6) 0.0034(5) 0.0062(5) 0.0040(5) N15 0.0109(6) 0.0209(7) 0.0104(6) 0.0011(5) 0.0030(5) 0.0002(5) N16 0.0146(7) 0.0192(6) 0.0193(7) -0.0004(5) 0.0086(6) 0.0009(5) N21 0.0093(6) 0.0124(6) 0.0109(6) -0.0005(5) 0.0028(5) -0.0022(5) N22 0.0099(6) 0.0129(6) 0.0101(6) 0.0020(5) 0.0026(5) 0.0001(5) N23 0.0116(6) 0.0126(6) 0.0129(6) -0.0006(5) 0.0055(5) 0.0007(5) N24 0.0105(6) 0.0125(6) 0.0137(6) -0.0001(5) 0.0034(5) -0.0032(5) N25 0.0109(6) 0.0129(6) 0.0104(6) 0.0018(5) 0.0027(5) -0.0019(5) N26 0.0138(7) 0.0171(6) 0.0136(7) -0.0026(5) 0.0064(6) 0.0000(5) C1 0.0085(7) 0.0243(8) 0.0156(8) 0.0056(6) 0.0043(6) 0.0019(6) C2 0.0130(8) 0.0274(8) 0.0163(8) 0.0069(6) 0.0080(7) 0.0073(6) C3 0.0106(7) 0.0227(8) 0.0096(7) 0.0028(6) 0.0021(6) 0.0027(6) C4 0.0092(7) 0.0222(8) 0.0121(7) 0.0012(6) 0.0002(6) 0.0008(6) C5 0.0113(8) 0.0208(8) 0.0155(8) 0.0033(6) 0.0043(6) 0.0051(6) C6 0.0158(8) 0.0191(7) 0.0172(8) 0.0031(6) 0.0063(7) 0.0030(6) C7 0.0101(7) 0.0180(7) 0.0151(8) 0.0010(6) 0.0047(6) -0.0023(6) C8 0.0102(8) 0.0155(7) 0.0163(8) -0.0005(6) 0.0011(6) -0.0024(6) C9 0.0107(8) 0.0194(7) 0.0122(7) 0.0023(6) 0.0017(6) -0.0001(6) C10 0.0119(8) 0.0160(7) 0.0127(7) 0.0035(6) 0.0034(6) 0.0015(6) C11 0.0123(8) 0.0163(7) 0.0177(8) -0.0018(6) 0.0047(7) 0.0018(6) C12 0.0125(8) 0.0231(8) 0.0164(8) -0.0040(6) 0.0055(7) 0.0018(6) C13 0.0095(7) 0.0165(7) 0.0099(7) -0.0011(5) 0.0018(6) -0.0002(6) C14 0.0101(7) 0.0138(7) 0.0085(7) -0.0009(5) 0.0033(6) 0.0002(5) C15 0.0217(9) 0.0228(8) 0.0142(8) 0.0037(6) 0.0095(7) 0.0020(7) C16 0.0201(9) 0.0256(8) 0.0145(8) 0.0064(6) 0.0055(7) 0.0061(7) C17 0.0130(8) 0.0259(8) 0.0126(8) 0.0017(6) 0.0030(6) 0.0047(6) C18 0.0180(8) 0.0225(8) 0.0166(8) -0.0028(6) 0.0080(7) 0.0000(6) C19 0.0163(8) 0.0217(8) 0.0222(9) 0.0010(7) 0.0083(7) 0.0033(6) C20 0.0121(8) 0.0214(8) 0.0172(8) 0.0044(6) 0.0047(7) 0.0030(6) C21 0.0209(9) 0.0216(8) 0.0363(11) -0.0078(7) 0.0160(8) -0.0034(7) C22 0.0173(9) 0.0332(10) 0.0321(11) -0.0154(8) 0.0088(8) -0.0038(7) C23 0.0142(8) 0.0335(9) 0.0175(9) -0.0075(7) 0.0049(7) 0.0018(7) C24 0.0200(9) 0.0111(7) 0.0185(8) 0.0004(6) 0.0060(7) -0.0028(6) C25 0.0194(9) 0.0141(7) 0.0176(8) 0.0031(6) 0.0057(7) 0.0024(6) C26 0.0123(8) 0.0149(7) 0.0125(7) 0.0017(6) 0.0030(6) 0.0008(6) C27 0.0154(8) 0.0183(7) 0.0115(7) 0.0004(6) 0.0057(6) -0.0047(6) C28 0.0187(8) 0.0200(8) 0.0162(8) -0.0015(6) 0.0101(7) -0.0014(6) C29 0.0155(8) 0.0165(7) 0.0152(8) 0.0007(6) 0.0070(7) 0.0021(6) C30 0.0230(9) 0.0229(8) 0.0140(8) -0.0050(6) 0.0085(7) -0.0019(7) C31 0.0240(9) 0.0238(8) 0.0117(8) -0.0010(6) 0.0049(7) -0.0005(7) C32 0.0165(8) 0.0172(7) 0.0143(8) 0.0013(6) 0.0031(7) 0.0016(6) O7 0.0971(18) 0.119(2) 0.0656(14) -0.0651(14) 0.0470(14) -0.0561(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 Cl2 2.2579(4) . ? Zn1 Cl3 2.2740(7) . ? Zn1 Cl1 2.2748(5) . ? Zn1 Cl4 2.2803(6) . ? Zn2 Cl7 2.2491(7) . ? Zn2 Cl5 2.2683(8) . ? Zn2 Cl8 2.2688(5) . ? Zn2 Cl6 2.3108(5) . ? Zn3 O23 2.0601(11) . ? Zn3 O3 2.0689(13) . ? Zn3 O4 2.0812(14) . ? Zn3 O13 2.0897(11) . ? Zn3 O1 2.0957(14) . ? Zn3 O2 2.1019(14) . ? Co1 O11 1.8990(12) . ? Co1 O12 1.9171(11) . ? Co1 N13 1.9285(15) . ? Co1 N11 1.9327(14) . ? Co1 N12 1.9447(14) . ? Co1 N1 2.0038(13) . ? Co1 C13 2.3212(16) . ? Co2 O21 1.8905(11) . ? Co2 N22 1.9124(14) . ? Co2 N21 1.9279(14) . ? Co2 O22 1.9291(11) . ? Co2 N23 1.9470(14) . ? Co2 N2 2.0092(13) . ? Co2 C14 2.3116(15) . ? O1 H92 0.81(3) . ? O1 H93 0.78(3) . ? O2 H88 0.82(3) . ? O2 H87 0.78(3) . ? O3 H89 0.89(3) . ? O3 H90 0.77(3) . ? O4 H85 0.80(2) . ? O4 H86 0.78(2) . ? O5 H83 0.77(3) . ? O5 H84 0.81(3) . ? O6 H81 0.74(3) . ? O6 H82 0.81(3) . ? O11 C13 1.3112(19) . ? O12 C13 1.3149(19) . ? O13 C13 1.2346(19) . ? O21 C14 1.3061(18) . ? O22 C14 1.3074(18) . ? O23 C14 1.2438(18) . ? N1 C1 1.507(2) . ? N1 C3 1.509(2) . ? N1 C5 1.512(2) . ? N2 C7 1.4969(19) . ? N2 C11 1.5040(19) . ? N2 C9 1.514(2) . ? N11 C17 1.338(2) . ? N11 N14 1.3540(19) . ? N12 C20 1.344(2) . ? N12 N15 1.3593(19) . ? N13 C23 1.339(2) . ? N13 N16 1.3547(19) . ? N14 C15 1.346(2) . ? N14 C2 1.457(2) . ? N15 C18 1.345(2) . ? N15 C4 1.455(2) . ? N16 C21 1.340(2) . ? N16 C6 1.452(2) . ? N21 C26 1.334(2) . ? N21 N24 1.3531(18) . ? N22 C29 1.339(2) . ? N22 N25 1.3526(17) . ? N23 C32 1.337(2) . ? N23 N26 1.3585(18) . ? N24 C24 1.347(2) . ? N24 C8 1.453(2) . ? N25 C27 1.341(2) . ? N25 C10 1.454(2) . ? N26 C30 1.343(2) . ? N26 C12 1.455(2) . ? C1 C2 1.513(2) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.507(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.515(2) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.509(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.504(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.505(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C15 C16 1.376(2) . ? C15 H15 0.9300 . ? C16 C17 1.387(2) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.373(2) . ? C18 H18 0.9300 . ? C19 C20 1.386(2) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.375(3) . ? C21 H21 0.9300 . ? C22 C23 1.389(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.368(2) . ? C24 H24 0.9300 . ? C25 C26 1.392(2) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.372(2) . ? C27 H27 0.9300 . ? C28 C29 1.389(2) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.372(2) . ? C30 H30 0.9300 . ? C31 C32 1.390(2) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Zn1 Cl3 109.52(2) . . ? Cl2 Zn1 Cl1 108.59(2) . . ? Cl3 Zn1 Cl1 113.23(2) . . ? Cl2 Zn1 Cl4 110.778(19) . . ? Cl3 Zn1 Cl4 106.57(2) . . ? Cl1 Zn1 Cl4 108.15(2) . . ? Cl7 Zn2 Cl5 114.64(2) . . ? Cl7 Zn2 Cl8 110.34(2) . . ? Cl5 Zn2 Cl8 111.94(2) . . ? Cl7 Zn2 Cl6 110.57(2) . . ? Cl5 Zn2 Cl6 104.18(2) . . ? Cl8 Zn2 Cl6 104.53(2) . . ? O23 Zn3 O3 86.99(5) . . ? O23 Zn3 O4 92.31(5) . . ? O3 Zn3 O4 85.81(5) . . ? O23 Zn3 O13 178.07(4) . . ? O3 Zn3 O13 93.68(5) . . ? O4 Zn3 O13 89.54(5) . . ? O23 Zn3 O1 89.29(5) . . ? O3 Zn3 O1 91.17(6) . . ? O4 Zn3 O1 176.50(6) . . ? O13 Zn3 O1 88.89(5) . . ? O23 Zn3 O2 90.29(5) . . ? O3 Zn3 O2 175.07(5) . . ? O4 Zn3 O2 90.20(5) . . ? O13 Zn3 O2 89.17(5) . . ? O1 Zn3 O2 92.91(6) . . ? O11 Co1 O12 68.89(5) . . ? O11 Co1 N13 88.90(6) . . ? O12 Co1 N13 87.05(5) . . ? O11 Co1 N11 165.10(5) . . ? O12 Co1 N11 96.23(5) . . ? N13 Co1 N11 91.04(6) . . ? O11 Co1 N12 88.71(5) . . ? O12 Co1 N12 87.74(5) . . ? N13 Co1 N12 174.77(6) . . ? N11 Co1 N12 90.08(6) . . ? O11 Co1 N1 97.15(5) . . ? O12 Co1 N1 166.04(5) . . ? N13 Co1 N1 92.77(6) . . ? N11 Co1 N1 97.73(6) . . ? N12 Co1 N1 92.15(6) . . ? O11 Co1 C13 34.39(5) . . ? O12 Co1 C13 34.51(5) . . ? N13 Co1 C13 87.09(6) . . ? N11 Co1 C13 130.73(6) . . ? N12 Co1 C13 88.31(5) . . ? N1 Co1 C13 131.54(5) . . ? O21 Co2 N22 89.16(5) . . ? O21 Co2 N21 165.80(5) . . ? N22 Co2 N21 88.66(5) . . ? O21 Co2 O22 68.80(4) . . ? N22 Co2 O22 86.51(5) . . ? N21 Co2 O22 97.06(5) . . ? O21 Co2 N23 88.90(5) . . ? N22 Co2 N23 174.25(6) . . ? N21 Co2 N23 91.91(5) . . ? O22 Co2 N23 87.74(5) . . ? O21 Co2 N2 97.01(5) . . ? N22 Co2 N2 92.76(5) . . ? N21 Co2 N2 97.11(5) . . ? O22 Co2 N2 165.79(5) . . ? N23 Co2 N2 92.85(5) . . ? O21 Co2 C14 34.40(5) . . ? N22 Co2 C14 86.14(5) . . ? N21 Co2 C14 131.41(5) . . ? O22 Co2 C14 34.44(5) . . ? N23 Co2 C14 89.20(5) . . ? N2 Co2 C14 131.36(5) . . ? Zn3 O1 H92 104.5(18) . . ? Zn3 O1 H93 110.8(19) . . ? H92 O1 H93 109(3) . . ? Zn3 O2 H88 122.0(18) . . ? Zn3 O2 H87 113(2) . . ? H88 O2 H87 110(3) . . ? Zn3 O3 H89 121.2(16) . . ? Zn3 O3 H90 117.9(18) . . ? H89 O3 H90 108(2) . . ? Zn3 O4 H85 133.4(17) . . ? Zn3 O4 H86 120.9(17) . . ? H85 O4 H86 105(2) . . ? H83 O5 H84 106(2) . . ? H81 O6 H82 107(3) . . ? C13 O11 Co1 90.72(9) . . ? C13 O12 Co1 89.81(9) . . ? C13 O13 Zn3 135.61(10) . . ? C14 O21 Co2 90.74(8) . . ? C14 O22 Co2 89.01(9) . . ? C14 O23 Zn3 135.34(10) . . ? C1 N1 C3 109.31(12) . . ? C1 N1 C5 106.87(12) . . ? C3 N1 C5 105.93(12) . . ? C1 N1 Co1 113.25(9) . . ? C3 N1 Co1 107.82(9) . . ? C5 N1 Co1 113.36(10) . . ? C7 N2 C11 109.27(12) . . ? C7 N2 C9 107.29(12) . . ? C11 N2 C9 105.55(12) . . ? C7 N2 Co2 111.70(9) . . ? C11 N2 Co2 107.53(9) . . ? C9 N2 Co2 115.24(9) . . ? C17 N11 N14 106.01(13) . . ? C17 N11 Co1 127.12(11) . . ? N14 N11 Co1 126.17(10) . . ? C20 N12 N15 105.60(13) . . ? C20 N12 Co1 125.42(11) . . ? N15 N12 Co1 126.20(10) . . ? C23 N13 N16 106.24(14) . . ? C23 N13 Co1 128.51(12) . . ? N16 N13 Co1 121.66(11) . . ? C15 N14 N11 110.65(13) . . ? C15 N14 C2 128.26(14) . . ? N11 N14 C2 120.40(13) . . ? C18 N15 N12 110.64(13) . . ? C18 N15 C4 125.42(14) . . ? N12 N15 C4 122.60(13) . . ? C21 N16 N13 110.55(15) . . ? C21 N16 C6 129.96(15) . . ? N13 N16 C6 119.31(13) . . ? C26 N21 N24 106.32(12) . . ? C26 N21 Co2 126.70(11) . . ? N24 N21 Co2 126.80(10) . . ? C29 N22 N25 106.28(12) . . ? C29 N22 Co2 129.45(11) . . ? N25 N22 Co2 123.35(10) . . ? C32 N23 N26 105.65(13) . . ? C32 N23 Co2 125.46(11) . . ? N26 N23 Co2 127.87(10) . . ? C24 N24 N21 110.40(13) . . ? C24 N24 C8 127.74(13) . . ? N21 N24 C8 121.31(12) . . ? C27 N25 N22 110.50(13) . . ? C27 N25 C10 129.24(13) . . ? N22 N25 C10 120.01(12) . . ? C30 N26 N23 110.56(13) . . ? C30 N26 C12 125.96(14) . . ? N23 N26 C12 122.96(13) . . ? N1 C1 C2 114.07(14) . . ? N1 C1 H1A 108.7 . . ? C2 C1 H1A 108.7 . . ? N1 C1 H1B 108.7 . . ? C2 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? N14 C2 C1 111.81(13) . . ? N14 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N14 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? C4 C3 N1 116.02(13) . . ? C4 C3 H3A 108.3 . . ? N1 C3 H3A 108.3 . . ? C4 C3 H3B 108.3 . . ? N1 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? N15 C4 C3 114.23(13) . . ? N15 C4 H4A 108.7 . . ? C3 C4 H4A 108.7 . . ? N15 C4 H4B 108.7 . . ? C3 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? N1 C5 C6 114.58(13) . . ? N1 C5 H5A 108.6 . . ? C6 C5 H5A 108.6 . . ? N1 C5 H5B 108.6 . . ? C6 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N16 C6 C5 109.19(13) . . ? N16 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? N16 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? N2 C7 C8 113.89(13) . . ? N2 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? N2 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N24 C8 C7 112.03(13) . . ? N24 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? N24 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C10 C9 N2 115.05(13) . . ? C10 C9 H9A 108.5 . . ? N2 C9 H9A 108.5 . . ? C10 C9 H9B 108.5 . . ? N2 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? N25 C10 C9 109.20(13) . . ? N25 C10 H10A 109.8 . . ? C9 C10 H10A 109.8 . . ? N25 C10 H10B 109.8 . . ? C9 C10 H10B 109.8 . . ? H10A C10 H10B 108.3 . . ? N2 C11 C12 116.36(13) . . ? N2 C11 H11A 108.2 . . ? C12 C11 H11A 108.2 . . ? N2 C11 H11B 108.2 . . ? C12 C11 H11B 108.2 . . ? H11A C11 H11B 107.3 . . ? N26 C12 C11 114.96(13) . . ? N26 C12 H12A 108.5 . . ? C11 C12 H12A 108.5 . . ? N26 C12 H12B 108.5 . . ? C11 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? O13 C13 O11 123.63(14) . . ? O13 C13 O12 125.81(14) . . ? O11 C13 O12 110.56(13) . . ? O13 C13 Co1 178.09(12) . . ? O11 C13 Co1 54.89(7) . . ? O12 C13 Co1 55.68(7) . . ? O23 C14 O21 122.38(13) . . ? O23 C14 O22 126.27(14) . . ? O21 C14 O22 111.33(13) . . ? O23 C14 Co2 175.44(12) . . ? O21 C14 Co2 54.86(7) . . ? O22 C14 Co2 56.55(7) . . ? N14 C15 C16 107.51(15) . . ? N14 C15 H15 126.2 . . ? C16 C15 H15 126.2 . . ? C15 C16 C17 105.38(15) . . ? C15 C16 H16 127.3 . . ? C17 C16 H16 127.3 . . ? N11 C17 C16 110.45(15) . . ? N11 C17 H17 124.8 . . ? C16 C17 H17 124.8 . . ? N15 C18 C19 107.76(15) . . ? N15 C18 H18 126.1 . . ? C19 C18 H18 126.1 . . ? C18 C19 C20 105.45(15) . . ? C18 C19 H19 127.3 . . ? C20 C19 H19 127.3 . . ? N12 C20 C19 110.52(15) . . ? N12 C20 H20 124.7 . . ? C19 C20 H20 124.7 . . ? N16 C21 C22 107.73(17) . . ? N16 C21 H21 126.1 . . ? C22 C21 H21 126.1 . . ? C21 C22 C23 105.49(16) . . ? C21 C22 H22 127.3 . . ? C23 C22 H22 127.3 . . ? N13 C23 C22 109.98(17) . . ? N13 C23 H23 125.0 . . ? C22 C23 H23 125.0 . . ? N24 C24 C25 107.68(14) . . ? N24 C24 H24 126.2 . . ? C25 C24 H24 126.2 . . ? C24 C25 C26 105.53(14) . . ? C24 C25 H25 127.2 . . ? C26 C25 H25 127.2 . . ? N21 C26 C25 110.07(14) . . ? N21 C26 H26 125.0 . . ? C25 C26 H26 125.0 . . ? N25 C27 C28 107.73(14) . . ? N25 C27 H27 126.1 . . ? C28 C27 H27 126.1 . . ? C27 C28 C29 105.57(14) . . ? C27 C28 H28 127.2 . . ? C29 C28 H28 127.2 . . ? N22 C29 C28 109.88(14) . . ? N22 C29 H29 125.1 . . ? C28 C29 H29 125.1 . . ? N26 C30 C31 108.02(15) . . ? N26 C30 H30 126.0 . . ? C31 C30 H30 126.0 . . ? C30 C31 C32 104.98(15) . . ? C30 C31 H31 127.5 . . ? C32 C31 H31 127.5 . . ? N23 C32 C31 110.77(15) . . ? N23 C32 H32 124.6 . . ? C31 C32 H32 124.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.863 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.072 #===END data_lme1r5 _database_code_depnum_ccdc_archive 'CCDC 686139' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H22 Cl4 Co N7 O3 Zn' _chemical_formula_weight 626.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 18.182(7) _cell_length_b 14.726(4) _cell_length_c 19.634(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5257(3) _cell_formula_units_Z 8 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 8266 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 32.65 _exptl_crystal_description rhombus _exptl_crystal_colour purple _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2528 _exptl_absorpt_coefficient_mu 1.981 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.792484 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SQUEEZE _exptl_special_details ; ? ; _diffrn_ambient_temperature 85(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa ApexII area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 119721 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 32.90 _reflns_number_total 9675 _reflns_number_gt 8143 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ApexII (Bruker, 2004)' _computing_cell_refinement 'ApexII and SAINT (Bruker, 2001)' _computing_data_reduction SAINT _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 1999)' _computing_publication_material WinGX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure was found to contain sigificant electron density which could not be reasonably assigned and was thought to indicate the presence of one or more disordered solvent molecules. The SQUEEZE option within PLATON generated a modified hkl file, which when used in subsequent least squares cycles, gave significantly improved R factors and, most importantly, a stable refinement. SQUEEZE gave an electron count of 198 per cell in a total void volume of 620.3 \%A^3^. Given that Z = 8, this corresponds to 19.8 disordered water molecules per cell, or approximately 2.5 water molecules per cation. The details of the SQUEEZE procedure are included at the end of this file. Disorder was present in the methylene arms of the trpyn ligand, and this was sucessfully modelled as an 84:16 ratio of two possible conformations of the methylene chains. The bicarbonate H atom was found in a search of the Fourier map and was allowed to refine freely. This led to a rather long O-H distance (1.14(4)\%A, but it was not considered necessary to introduce a restraint to reduce this to a more realistic value. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+7.9014P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9675 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.1034 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.794081(15) -0.143437(18) 0.485467(12) 0.02726(7) Uani 1 1 d . . . Co1 Co 0.895130(13) 0.133271(16) 0.709387(12) 0.01449(6) Uani 1 1 d . A . Cl1 Cl 0.89400(3) -0.22829(5) 0.51158(3) 0.04045(14) Uani 1 1 d . . . Cl2 Cl 0.82764(5) -0.02468(5) 0.41843(3) 0.0555(2) Uani 1 1 d . . . Cl3 Cl 0.73726(3) -0.09789(4) 0.58249(3) 0.03246(12) Uani 1 1 d . . . Cl4 Cl 0.71222(3) -0.23328(4) 0.42748(3) 0.02961(11) Uani 1 1 d . . . N1 N 0.91437(9) 0.13527(10) 0.60969(8) 0.0185(3) Uani 1 1 d . . . N11 N 0.79051(8) 0.13415(10) 0.70424(8) 0.0164(3) Uani 1 1 d . . . N12 N 0.74837(8) 0.13650(11) 0.64769(8) 0.0179(3) Uani 1 1 d . A . N21 N 0.89437(10) 0.00218(11) 0.71034(9) 0.0226(3) Uani 1 1 d . . . N22 N 0.92982(10) -0.05516(12) 0.66719(10) 0.0268(3) Uani 1 1 d . A . N31 N 0.89582(9) 0.26347(11) 0.71756(8) 0.0199(3) Uani 1 1 d . . . N32 N 0.93906(9) 0.31972(11) 0.68098(9) 0.0221(3) Uani 1 1 d . A . O1 O 0.99515(8) 0.13227(11) 0.74244(8) 0.0252(3) Uani 1 1 d . . . O2 O 0.89791(7) 0.12893(9) 0.80656(7) 0.0178(2) Uani 1 1 d . . . O3 O 1.00979(9) 0.12886(14) 0.85576(9) 0.0367(4) Uani 1 1 d . . . C1 C 0.84997(13) 0.09993(17) 0.56947(11) 0.0226(5) Uani 0.843(4) 1 d P A 1 H1A H 0.8623 0.1028 0.5214 0.027 Uiso 0.843(4) 1 calc PR A 1 H1B H 0.8428 0.0365 0.5810 0.027 Uiso 0.843(4) 1 calc PR A 1 C3 C 0.97987(13) 0.07678(16) 0.59747(12) 0.0236(5) Uani 0.843(4) 1 d P A 1 H3A H 1.0182 0.0946 0.6291 0.028 Uiso 0.843(4) 1 calc PR A 1 H3B H 0.9979 0.0886 0.5518 0.028 Uiso 0.843(4) 1 calc PR A 1 C5 C 0.93266(13) 0.22817(16) 0.58000(11) 0.0230(5) Uani 0.843(4) 1 d P A 1 H5A H 0.9562 0.2197 0.5361 0.028 Uiso 0.843(4) 1 calc PR A 1 H5B H 0.8872 0.2610 0.5723 0.028 Uiso 0.843(4) 1 calc PR A 1 C1' C 0.8564(7) 0.1762(7) 0.5750(5) 0.018(2) Uani 0.157(4) 1 d P A 2 H11 H 0.8689 0.1730 0.5271 0.021 Uiso 0.157(4) 1 calc PR A 2 H12 H 0.8579 0.2400 0.5873 0.021 Uiso 0.157(4) 1 calc PR A 2 C3' C 0.9283(7) 0.0385(8) 0.5829(6) 0.021(2) Uani 0.157(4) 1 d P A 2 H31 H 0.8796 0.0123 0.5788 0.026 Uiso 0.157(4) 1 calc PR A 2 H32 H 0.9454 0.0476 0.5366 0.026 Uiso 0.157(4) 1 calc PR A 2 C5' C 0.9869(6) 0.1838(9) 0.6075(6) 0.022(2) Uani 0.157(4) 1 d P A 2 H51 H 1.0080 0.1767 0.5625 0.026 Uiso 0.157(4) 1 calc PR A 2 H52 H 1.0201 0.1554 0.6398 0.026 Uiso 0.157(4) 1 calc PR A 2 C2 C 0.77912(11) 0.14868(16) 0.58014(10) 0.0264(4) Uani 1 1 d . . . H2A H 0.7869 0.2130 0.5723 0.032 Uiso 1 1 calc R A 1 H2B H 0.7438 0.1274 0.5468 0.032 Uiso 1 1 calc R A 1 C4 C 0.96702(14) -0.02506(16) 0.60476(15) 0.0361(5) Uani 1 1 d . . . H4A H 0.9382 -0.0453 0.5661 0.043 Uiso 1 1 calc R A 1 H4B H 1.0143 -0.0554 0.6023 0.043 Uiso 1 1 calc R A 1 C6 C 0.98165(12) 0.28474(14) 0.62395(11) 0.0251(4) Uani 1 1 d . . . H6A H 1.0222 0.2483 0.6407 0.030 Uiso 1 1 calc R A 1 H6B H 1.0017 0.3347 0.5977 0.030 Uiso 1 1 calc R A 1 C7 C 0.96878(10) 0.13008(14) 0.80348(10) 0.0228(4) Uani 1 1 d . A . C13 C 0.67652(10) 0.13345(14) 0.66432(11) 0.0234(4) Uani 1 1 d . . . H13 H 0.6372 0.1346 0.6341 0.028 Uiso 1 1 calc R A . C14 C 0.67201(10) 0.12832(13) 0.73404(11) 0.0226(3) Uani 1 1 d . A . H14 H 0.6294 0.1250 0.7602 0.027 Uiso 1 1 calc R . . C15 C 0.74441(10) 0.12904(13) 0.75756(10) 0.0196(3) Uani 1 1 d . A . H15 H 0.7585 0.1264 0.8030 0.024 Uiso 1 1 calc R . . C23 C 0.91804(14) -0.14222(14) 0.68672(14) 0.0342(5) Uani 1 1 d . . . H23 H 0.9356 -0.1937 0.6647 0.041 Uiso 1 1 calc R A . C24 C 0.87626(16) -0.14136(15) 0.74389(13) 0.0346(5) Uani 1 1 d . A . H24 H 0.8603 -0.1912 0.7689 0.042 Uiso 1 1 calc R . . C25 C 0.86234(14) -0.04985(14) 0.75726(11) 0.0289(4) Uani 1 1 d . A . H25 H 0.8347 -0.0283 0.7937 0.035 Uiso 1 1 calc R . . C33 C 0.93186(14) 0.40577(15) 0.70291(12) 0.0305(4) Uani 1 1 d . . . H33 H 0.9553 0.4565 0.6850 0.037 Uiso 1 1 calc R A . C34 C 0.88354(15) 0.40501(14) 0.75664(12) 0.0320(5) Uani 1 1 d . A . H34 H 0.8684 0.4544 0.7826 0.038 Uiso 1 1 calc R . . C35 C 0.86202(13) 0.31480(14) 0.76415(11) 0.0261(4) Uani 1 1 d . A . H35 H 0.8291 0.2935 0.7967 0.031 Uiso 1 1 calc R . . H60 H 0.974(2) 0.133(3) 0.904(2) 0.067(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02895(13) 0.03473(13) 0.01811(11) 0.00045(9) 0.00276(9) -0.01120(10) Co1 0.01131(10) 0.01807(10) 0.01409(10) -0.00285(8) -0.00007(7) 0.00028(7) Cl1 0.0262(2) 0.0615(4) 0.0336(3) -0.0058(3) 0.0017(2) -0.0027(2) Cl2 0.0896(6) 0.0513(4) 0.0258(3) 0.0029(3) 0.0113(3) -0.0404(4) Cl3 0.0388(3) 0.0342(3) 0.0244(2) -0.00569(19) 0.0080(2) -0.0121(2) Cl4 0.0355(3) 0.0314(2) 0.0219(2) 0.00239(18) -0.01039(18) -0.00465(19) N1 0.0174(6) 0.0209(7) 0.0171(6) -0.0027(5) 0.0024(5) -0.0032(5) N11 0.0130(6) 0.0219(7) 0.0143(6) 0.0004(5) -0.0023(5) -0.0001(5) N12 0.0134(6) 0.0226(7) 0.0177(6) 0.0002(5) -0.0040(5) 0.0003(5) N21 0.0264(8) 0.0185(7) 0.0229(7) -0.0045(6) -0.0034(6) 0.0036(6) N22 0.0261(8) 0.0211(7) 0.0331(9) -0.0094(6) -0.0029(7) 0.0040(6) N31 0.0228(7) 0.0188(7) 0.0181(7) -0.0006(5) 0.0023(6) -0.0028(5) N32 0.0239(7) 0.0205(7) 0.0218(7) 0.0010(6) 0.0003(6) -0.0062(6) O1 0.0119(5) 0.0408(8) 0.0227(7) -0.0087(6) -0.0003(5) 0.0021(5) O2 0.0154(5) 0.0230(6) 0.0150(5) -0.0026(4) -0.0023(4) 0.0023(4) O3 0.0200(7) 0.0663(12) 0.0237(7) -0.0118(7) -0.0093(6) 0.0078(7) C1 0.0233(10) 0.0302(11) 0.0143(9) -0.0033(8) -0.0018(7) -0.0056(8) C3 0.0225(10) 0.0270(10) 0.0213(10) -0.0051(8) 0.0065(8) 0.0001(8) C5 0.0264(11) 0.0250(10) 0.0177(9) 0.0026(8) 0.0023(8) -0.0059(8) C1' 0.027(5) 0.016(4) 0.010(4) 0.002(3) 0.003(4) 0.004(4) C3' 0.029(6) 0.022(5) 0.013(4) 0.001(4) 0.006(4) 0.007(4) C5' 0.009(4) 0.035(6) 0.021(5) -0.005(5) 0.006(4) -0.004(4) C2 0.0225(9) 0.0411(11) 0.0157(8) 0.0047(7) -0.0044(6) -0.0053(8) C4 0.0302(11) 0.0286(10) 0.0496(14) -0.0104(10) 0.0111(10) 0.0021(8) C6 0.0255(9) 0.0250(8) 0.0249(9) 0.0003(7) 0.0046(7) -0.0078(7) C7 0.0163(8) 0.0304(9) 0.0218(8) -0.0074(7) -0.0048(6) 0.0055(6) C13 0.0125(7) 0.0291(9) 0.0286(9) -0.0015(7) -0.0045(6) 0.0018(6) C14 0.0125(7) 0.0268(8) 0.0284(9) -0.0010(7) 0.0025(6) 0.0002(6) C15 0.0125(7) 0.0260(8) 0.0205(8) 0.0007(6) 0.0024(6) 0.0004(6) C23 0.0382(12) 0.0192(9) 0.0451(13) -0.0080(8) -0.0098(10) 0.0061(8) C24 0.0479(14) 0.0204(9) 0.0357(12) 0.0008(8) -0.0116(10) 0.0004(8) C25 0.0396(12) 0.0216(8) 0.0257(9) 0.0003(7) -0.0036(8) 0.0008(8) C33 0.0371(11) 0.0215(9) 0.0330(11) -0.0001(8) -0.0042(9) -0.0051(8) C34 0.0449(13) 0.0207(9) 0.0305(10) -0.0038(8) -0.0021(9) 0.0008(8) C35 0.0341(10) 0.0218(8) 0.0224(9) -0.0032(7) 0.0035(8) 0.0023(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 Cl1 2.2638(9) . ? Zn1 Cl3 2.2685(8) . ? Zn1 Cl2 2.2722(8) . ? Zn1 Cl4 2.2939(7) . ? Co1 N11 1.9050(16) . ? Co1 O2 1.9096(15) . ? Co1 N31 1.9239(17) . ? Co1 N21 1.9305(17) . ? Co1 O1 1.9310(15) . ? Co1 N1 1.9887(17) . ? Co1 C7 2.282(2) . ? N1 C1' 1.391(11) . ? N1 C3 1.489(3) . ? N1 C5' 1.501(11) . ? N1 C1 1.505(3) . ? N1 C5 1.524(3) . ? N1 C3' 1.540(12) . ? N11 C15 1.343(2) . ? N11 N12 1.349(2) . ? N12 C13 1.347(2) . ? N12 C2 1.451(3) . ? N21 C25 1.332(3) . ? N21 N22 1.359(2) . ? N22 C23 1.355(3) . ? N22 C4 1.468(3) . ? N31 C35 1.336(3) . ? N31 N32 1.349(2) . ? N32 C33 1.345(3) . ? N32 C6 1.456(3) . ? O1 C7 1.291(3) . ? O2 C7 1.290(2) . ? O3 C7 1.269(2) . ? O3 H60 1.14(4) . ? C1 C2 1.489(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C3 C4 1.524(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 C6 1.494(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C1' C2 1.466(12) . ? C1' H11 0.9700 . ? C1' H12 0.9700 . ? C3' C4 1.248(12) . ? C3' H31 0.9700 . ? C3' H32 0.9700 . ? C5' C6 1.524(13) . ? C5' H51 0.9700 . ? C5' H52 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C13 C14 1.373(3) . ? C13 H13 0.9300 . ? C14 C15 1.395(3) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C23 C24 1.355(4) . ? C23 H23 0.9300 . ? C24 C25 1.396(3) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C33 C34 1.373(4) . ? C33 H33 0.9300 . ? C34 C35 1.393(3) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Zn1 Cl3 109.78(3) . . ? Cl1 Zn1 Cl2 109.91(4) . . ? Cl3 Zn1 Cl2 112.41(3) . . ? Cl1 Zn1 Cl4 108.34(3) . . ? Cl3 Zn1 Cl4 106.97(3) . . ? Cl2 Zn1 Cl4 109.31(3) . . ? N11 Co1 O2 94.57(6) . . ? N11 Co1 N31 90.24(7) . . ? O2 Co1 N31 87.13(6) . . ? N11 Co1 N21 90.01(7) . . ? O2 Co1 N21 87.54(6) . . ? N31 Co1 N21 174.66(7) . . ? N11 Co1 O1 163.40(7) . . ? O2 Co1 O1 68.84(6) . . ? N31 Co1 O1 88.48(7) . . ? N21 Co1 O1 89.76(7) . . ? N11 Co1 N1 97.08(7) . . ? O2 Co1 N1 168.31(6) . . ? N31 Co1 N1 93.80(7) . . ? N21 Co1 N1 91.47(7) . . ? O1 Co1 N1 99.51(7) . . ? N11 Co1 C7 128.98(7) . . ? O2 Co1 C7 34.41(6) . . ? N31 Co1 C7 87.09(7) . . ? N21 Co1 C7 88.61(7) . . ? O1 Co1 C7 34.43(7) . . ? N1 Co1 C7 133.94(7) . . ? C1' N1 C3 141.0(5) . . ? C1' N1 C5' 116.5(7) . . ? C3 N1 C5' 64.4(5) . . ? C1' N1 C1 45.9(5) . . ? C3 N1 C1 109.74(16) . . ? C5' N1 C1 146.5(5) . . ? C1' N1 C5 65.8(5) . . ? C3 N1 C5 106.44(16) . . ? C5' N1 C5 50.9(5) . . ? C1 N1 C5 106.23(16) . . ? C1' N1 C3' 111.0(7) . . ? C3 N1 C3' 43.8(5) . . ? C5' N1 C3' 106.6(7) . . ? C1 N1 C3' 68.2(5) . . ? C5 N1 C3' 131.6(5) . . ? C1' N1 Co1 110.8(4) . . ? C3 N1 Co1 106.90(13) . . ? C5' N1 Co1 100.9(5) . . ? C1 N1 Co1 111.99(12) . . ? C5 N1 Co1 115.35(12) . . ? C3' N1 Co1 110.6(4) . . ? C15 N11 N12 106.76(15) . . ? C15 N11 Co1 125.55(12) . . ? N12 N11 Co1 127.65(12) . . ? C13 N12 N11 110.50(16) . . ? C13 N12 C2 126.83(16) . . ? N11 N12 C2 122.46(15) . . ? C25 N21 N22 106.33(17) . . ? C25 N21 Co1 125.80(14) . . ? N22 N21 Co1 127.73(14) . . ? C23 N22 N21 109.7(2) . . ? C23 N22 C4 126.48(19) . . ? N21 N22 C4 123.46(18) . . ? C35 N31 N32 106.56(16) . . ? C35 N31 Co1 128.15(14) . . ? N32 N31 Co1 124.84(13) . . ? C33 N32 N31 110.57(17) . . ? C33 N32 C6 129.16(18) . . ? N31 N32 C6 120.15(16) . . ? C7 O1 Co1 87.85(11) . . ? C7 O2 Co1 88.81(11) . . ? C7 O3 H60 109(2) . . ? C2 C1 N1 115.62(18) . . ? C2 C1 H1A 108.4 . . ? N1 C1 H1A 108.4 . . ? C2 C1 H1B 108.4 . . ? N1 C1 H1B 108.4 . . ? H1A C1 H1B 107.4 . . ? N1 C3 C4 115.54(19) . . ? N1 C3 H3A 108.4 . . ? C4 C3 H3A 108.4 . . ? N1 C3 H3B 108.4 . . ? C4 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? C6 C5 N1 114.19(18) . . ? C6 C5 H5A 108.7 . . ? N1 C5 H5A 108.7 . . ? C6 C5 H5B 108.7 . . ? N1 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N1 C1' C2 124.9(8) . . ? N1 C1' H11 106.1 . . ? C2 C1' H11 106.1 . . ? N1 C1' H12 106.1 . . ? C2 C1' H12 106.1 . . ? H11 C1' H12 106.3 . . ? C4 C3' N1 132.0(10) . . ? C4 C3' H31 104.2 . . ? N1 C3' H31 104.2 . . ? C4 C3' H32 104.2 . . ? N1 C3' H32 104.2 . . ? H31 C3' H32 105.5 . . ? N1 C5' C6 113.8(7) . . ? N1 C5' H51 108.8 . . ? C6 C5' H51 108.8 . . ? N1 C5' H52 108.8 . . ? C6 C5' H52 108.8 . . ? H51 C5' H52 107.7 . . ? N12 C2 C1' 117.8(4) . . ? N12 C2 C1 113.72(17) . . ? C1' C2 C1 45.1(4) . . ? N12 C2 H2A 108.8 . . ? C1' C2 H2A 65.2 . . ? C1 C2 H2A 108.8 . . ? N12 C2 H2B 108.8 . . ? C1' C2 H2B 132.7 . . ? C1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C3' C4 N22 104.7(6) . . ? C3' C4 C3 46.8(6) . . ? N22 C4 C3 116.49(19) . . ? C3' C4 H4A 69.9 . . ? N22 C4 H4A 108.2 . . ? C3 C4 H4A 108.2 . . ? C3' C4 H4B 145.9 . . ? N22 C4 H4B 108.2 . . ? C3 C4 H4B 108.2 . . ? H4A C4 H4B 107.3 . . ? N32 C6 C5 108.93(17) . . ? N32 C6 C5' 122.8(4) . . ? C5 C6 C5' 51.1(5) . . ? N32 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? C5' C6 H6A 58.9 . . ? N32 C6 H6B 109.9 . . ? C5 C6 H6B 109.9 . . ? C5' C6 H6B 127.2 . . ? H6A C6 H6B 108.3 . . ? O3 C7 O2 123.29(19) . . ? O3 C7 O1 122.22(18) . . ? O2 C7 O1 114.50(16) . . ? O3 C7 Co1 179.63(19) . . ? O2 C7 Co1 56.78(9) . . ? O1 C7 Co1 57.72(10) . . ? N12 C13 C14 107.53(16) . . ? N12 C13 H13 126.2 . . ? C14 C13 H13 126.2 . . ? C13 C14 C15 105.85(17) . . ? C13 C14 H14 127.1 . . ? C15 C14 H14 127.1 . . ? N11 C15 C14 109.35(17) . . ? N11 C15 H15 125.3 . . ? C14 C15 H15 125.3 . . ? N22 C23 C24 108.31(19) . . ? N22 C23 H23 125.8 . . ? C24 C23 H23 125.8 . . ? C23 C24 C25 105.4(2) . . ? C23 C24 H24 127.3 . . ? C25 C24 H24 127.3 . . ? N21 C25 C24 110.2(2) . . ? N21 C25 H25 124.9 . . ? C24 C25 H25 124.9 . . ? N32 C33 C34 107.50(19) . . ? N32 C33 H33 126.3 . . ? C34 C33 H33 126.3 . . ? C33 C34 C35 105.60(19) . . ? C33 C34 H34 127.2 . . ? C35 C34 H34 127.2 . . ? N31 C35 C34 109.75(19) . . ? N31 C35 H35 125.1 . . ? C34 C35 H35 125.1 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.310 _refine_diff_density_min -1.249 _refine_diff_density_rms 0.093 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 152.6 49.2 2 0.500 0.000 0.500 152.5 49.5 3 0.000 0.500 0.500 152.6 49.6 4 0.500 0.500 1.000 152.6 49.9 _platon_squeeze_details ; ? ; #===END data_trpyn _database_code_depnum_ccdc_archive 'CCDC 686140' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H21 Cl Co N7 O7' _chemical_formula_weight 517.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2764(4) _cell_length_b 11.9332(3) _cell_length_c 27.9535(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.0820(10) _cell_angle_gamma 90.00 _cell_volume 4031.9(2) _cell_formula_units_Z 8 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 9238 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 33.10 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 1.042 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.843241 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 85(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa ApexII area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 83629 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 33.37 _reflns_number_total 12412 _reflns_number_gt 10840 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ApexII (Bruker, 2004)' _computing_cell_refinement 'ApexII and SAINT (Bruker, 2001)' _computing_data_reduction SAINT _computing_structure_solution 'SIR2004 (Burla et al., 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 1999)' _computing_publication_material WinGX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+8.2224P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12412 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.1130 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.24196(2) 0.11429(2) 0.929095(9) 0.01017(6) Uani 1 1 d . . . Co2 Co 0.65217(2) 0.54665(2) 0.821863(10) 0.01296(6) Uani 1 1 d . . . Cl1 Cl 0.12773(4) 0.60556(4) 0.963757(17) 0.01796(10) Uani 1 1 d . . . Cl2 Cl 0.36045(4) 0.19373(4) 0.716839(17) 0.01586(9) Uani 1 1 d . . . O1 O 0.13951(17) 0.62014(16) 0.91366(6) 0.0287(4) Uani 1 1 d . . . O2 O 0.10615(16) 0.48928(14) 0.97237(7) 0.0282(4) Uani 1 1 d . . . O3 O 0.03367(18) 0.67158(16) 0.97164(8) 0.0343(4) Uani 1 1 d . . . O4 O 0.2257(2) 0.6419(3) 0.99516(9) 0.0604(8) Uani 1 1 d . . . O5 O 0.34770(15) 0.27740(15) 0.75266(6) 0.0260(3) Uani 1 1 d . . . O6 O 0.25468(14) 0.17614(16) 0.68605(7) 0.0283(4) Uani 1 1 d . . . O7 O 0.43989(14) 0.23217(17) 0.68836(6) 0.0290(4) Uani 1 1 d . . . O8 O 0.39817(16) 0.09004(15) 0.74072(7) 0.0292(4) Uani 1 1 d . . . O12 O 0.25361(12) 0.21162(12) 0.98344(5) 0.0144(3) Uani 1 1 d . . . O11 O 0.28501(12) 0.03330(12) 0.98769(5) 0.0135(3) Uani 1 1 d . . . O13 O 0.29830(12) 0.13085(13) 1.05785(5) 0.0168(3) Uani 1 1 d . . . O21 O 0.53553(11) 0.52625(12) 0.76783(5) 0.0140(3) Uani 1 1 d . . . O22 O 0.70824(12) 0.54686(13) 0.76307(5) 0.0182(3) Uani 1 1 d . . . O23 O 0.58716(13) 0.52025(14) 0.69352(6) 0.0191(3) Uani 1 1 d . . . N1 N 0.23982(13) -0.01518(14) 0.88288(6) 0.0124(3) Uani 1 1 d . . . N2 N 0.79736(15) 0.57001(15) 0.86652(7) 0.0190(3) Uani 1 1 d . . . N11 N 0.19880(14) 0.22894(14) 0.88105(6) 0.0138(3) Uani 1 1 d . . . N12 N 0.18921(14) 0.21908(15) 0.83241(6) 0.0146(3) Uani 1 1 d . . . N21 N 0.08794(13) 0.09250(14) 0.93429(6) 0.0134(3) Uani 1 1 d . . . N22 N 0.02706(14) -0.00231(15) 0.92595(6) 0.0156(3) Uani 1 1 d . . . N31 N 0.39452(13) 0.14745(15) 0.92750(6) 0.0139(3) Uani 1 1 d . . . N32 N 0.47362(14) 0.06790(15) 0.92861(6) 0.0156(3) Uani 1 1 d . . . N41 N 0.55910(15) 0.54290(14) 0.87118(6) 0.0157(3) Uani 1 1 d . . . N42 N 0.59021(17) 0.57016(16) 0.91855(7) 0.0202(4) Uani 1 1 d . . . N51 N 0.66966(16) 0.38556(15) 0.82520(7) 0.0199(4) Uani 1 1 d . . . N52 N 0.76531(16) 0.32615(16) 0.83283(7) 0.0218(4) Uani 1 1 d . . . N61 N 0.62475(13) 0.70547(14) 0.81483(6) 0.0137(3) Uani 1 1 d . . . N62 N 0.70381(15) 0.78068(15) 0.80909(7) 0.0188(3) Uani 1 1 d . . . C1 C 0.28067(15) 0.12635(17) 1.01320(7) 0.0135(3) Uani 1 1 d . . . C2 C 0.60743(16) 0.53021(17) 0.73796(7) 0.0153(3) Uani 1 1 d . . . C11 C 0.17415(18) 0.01180(18) 0.83368(7) 0.0177(4) Uani 1 1 d . . . H11A H 0.0975 0.0232 0.8369 0.021 Uiso 1 1 calc R . . H11B H 0.1767 -0.0522 0.8125 0.021 Uiso 1 1 calc R . . C12 C 0.2136(2) 0.11371(18) 0.80987(8) 0.0199(4) Uani 1 1 d . . . H12A H 0.2929 0.1080 0.8113 0.024 Uiso 1 1 calc R . . H12B H 0.1790 0.1148 0.7759 0.024 Uiso 1 1 calc R . . C13 C 0.16690(19) 0.31952(19) 0.81071(8) 0.0201(4) Uani 1 1 d . . . H13 H 0.1574 0.3337 0.7775 0.024 Uiso 1 1 calc R . . C14 C 0.1608(2) 0.39717(18) 0.84651(8) 0.0216(4) Uani 1 1 d . . . H14 H 0.1461 0.4734 0.8426 0.026 Uiso 1 1 calc R . . C15 C 0.18113(17) 0.33707(17) 0.88997(8) 0.0176(4) Uani 1 1 d . . . H15 H 0.1823 0.3676 0.9207 0.021 Uiso 1 1 calc R . . C21 C 0.18631(17) -0.11187(17) 0.90491(8) 0.0174(4) Uani 1 1 d . . . H21A H 0.2011 -0.1801 0.8883 0.021 Uiso 1 1 calc R . . H21B H 0.2214 -0.1193 0.9387 0.021 Uiso 1 1 calc R . . C22 C 0.06336(18) -0.10245(18) 0.90288(8) 0.0188(4) Uani 1 1 d . . . H22A H 0.0275 -0.1034 0.8691 0.023 Uiso 1 1 calc R . . H22B H 0.0383 -0.1680 0.9184 0.023 Uiso 1 1 calc R . . C23 C -0.07455(17) 0.0135(2) 0.93662(8) 0.0221(4) Uani 1 1 d . . . H23 H -0.1311 -0.0393 0.9334 0.026 Uiso 1 1 calc R . . C24 C -0.08000(18) 0.1217(2) 0.95323(8) 0.0224(4) Uani 1 1 d . . . H24 H -0.1397 0.1563 0.9635 0.027 Uiso 1 1 calc R . . C25 C 0.02318(17) 0.16797(19) 0.95131(8) 0.0181(4) Uani 1 1 d . . . H25 H 0.0443 0.2408 0.9605 0.022 Uiso 1 1 calc R . . C31 C 0.35177(17) -0.05642(19) 0.87607(8) 0.0200(4) Uani 1 1 d . . . H31A H 0.3753 -0.0133 0.8503 0.024 Uiso 1 1 calc R . . H31B H 0.3450 -0.1340 0.8655 0.024 Uiso 1 1 calc R . . C32 C 0.44055(17) -0.04897(18) 0.92086(8) 0.0195(4) Uani 1 1 d . . . H32A H 0.4124 -0.0772 0.9489 0.023 Uiso 1 1 calc R . . H32B H 0.5038 -0.0941 0.9165 0.023 Uiso 1 1 calc R . . C33 C 0.57488(17) 0.1149(2) 0.93357(8) 0.0205(4) Uani 1 1 d . . . H33 H 0.6416 0.0772 0.9347 0.025 Uiso 1 1 calc R . . C34 C 0.56121(18) 0.2292(2) 0.93660(9) 0.0246(5) Uani 1 1 d . . . H34 H 0.6162 0.2837 0.9406 0.029 Uiso 1 1 calc R . . C35 C 0.44770(18) 0.24584(19) 0.93248(8) 0.0196(4) Uani 1 1 d . . . H35 H 0.4137 0.3153 0.9331 0.024 Uiso 1 1 calc R . . C41 C 0.7926(2) 0.5362(2) 0.91595(9) 0.0272(5) Uani 1 1 d . . . H41A H 0.8647 0.5489 0.9358 0.033 Uiso 1 1 calc R . . H41B H 0.7780 0.4564 0.9161 0.033 Uiso 1 1 calc R . . C42 C 0.7065(2) 0.5959(3) 0.93930(9) 0.0328(6) Uani 1 1 d . . . H42A H 0.7190 0.5771 0.9736 0.039 Uiso 1 1 calc R . . H42B H 0.7176 0.6760 0.9368 0.039 Uiso 1 1 calc R . . C43 C 0.5008(2) 0.5801(2) 0.93991(9) 0.0288(5) Uani 1 1 d . . . H43 H 0.5013 0.5991 0.9722 0.035 Uiso 1 1 calc R . . C44 C 0.4084(2) 0.5572(2) 0.90579(9) 0.0297(5) Uani 1 1 d . . . H44 H 0.3350 0.5572 0.9101 0.036 Uiso 1 1 calc R . . C45 C 0.44896(18) 0.53424(19) 0.86327(8) 0.0206(4) Uani 1 1 d . . . H45 H 0.4055 0.5156 0.8337 0.025 Uiso 1 1 calc R . . C51 C 0.8843(2) 0.5011(2) 0.84619(10) 0.0283(5) Uani 1 1 d . . . H51A H 0.8789 0.5179 0.8119 0.034 Uiso 1 1 calc R . . H51B H 0.9573 0.5235 0.8625 0.034 Uiso 1 1 calc R . . C52 C 0.8717(2) 0.37570(19) 0.85223(9) 0.0238(4) Uani 1 1 d . . . H52A H 0.9272 0.3387 0.8371 0.029 Uiso 1 1 calc R . . H52B H 0.8884 0.3588 0.8867 0.029 Uiso 1 1 calc R . . C53 C 0.7439(2) 0.2157(2) 0.82517(9) 0.0277(5) Uani 1 1 d . . . H53 H 0.7960 0.1584 0.8287 0.033 Uiso 1 1 calc R . . C54 C 0.6322(2) 0.2033(2) 0.81129(10) 0.0294(5) Uani 1 1 d . . . H54 H 0.5935 0.1370 0.8033 0.035 Uiso 1 1 calc R . . C55 C 0.5887(2) 0.31133(19) 0.81164(9) 0.0251(5) Uani 1 1 d . . . H55 H 0.5140 0.3291 0.8036 0.030 Uiso 1 1 calc R . . C61 C 0.8419(2) 0.6898(2) 0.86579(9) 0.0273(5) Uani 1 1 d . . . H61A H 0.8112 0.7337 0.8894 0.033 Uiso 1 1 calc R . . H61B H 0.9215 0.6875 0.8764 0.033 Uiso 1 1 calc R . . C62 C 0.81857(19) 0.7492(2) 0.81824(11) 0.0282(5) Uani 1 1 d . . . H62A H 0.8648 0.8154 0.8192 0.034 Uiso 1 1 calc R . . H62B H 0.8345 0.7005 0.7925 0.034 Uiso 1 1 calc R . . C63 C 0.6596(2) 0.88157(18) 0.79670(9) 0.0219(4) Uani 1 1 d . . . H63 H 0.6980 0.9462 0.7914 0.026 Uiso 1 1 calc R . . C64 C 0.54688(19) 0.87183(18) 0.79324(9) 0.0218(4) Uani 1 1 d . . . H64 H 0.4941 0.9277 0.7850 0.026 Uiso 1 1 calc R . . C65 C 0.52836(17) 0.76002(17) 0.80472(8) 0.0168(4) Uani 1 1 d . . . H65 H 0.4593 0.7284 0.8052 0.020 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01007(11) 0.00966(12) 0.01030(11) -0.00053(8) 0.00043(8) -0.00009(8) Co2 0.01044(11) 0.01116(12) 0.01575(12) -0.00447(9) -0.00190(9) 0.00197(9) Cl1 0.0202(2) 0.0178(2) 0.0158(2) 0.00240(16) 0.00288(16) -0.00227(17) Cl2 0.01477(19) 0.0163(2) 0.0166(2) 0.00109(16) 0.00312(15) 0.00020(16) O1 0.0400(10) 0.0282(9) 0.0205(8) 0.0041(7) 0.0126(7) 0.0010(8) O2 0.0374(10) 0.0163(7) 0.0336(9) 0.0069(7) 0.0140(8) 0.0046(7) O3 0.0449(11) 0.0215(8) 0.0423(11) 0.0016(8) 0.0233(9) 0.0069(8) O4 0.0426(13) 0.085(2) 0.0436(13) 0.0089(13) -0.0196(10) -0.0351(13) O5 0.0300(8) 0.0203(8) 0.0289(8) -0.0074(7) 0.0083(7) -0.0027(7) O6 0.0170(7) 0.0352(10) 0.0299(9) -0.0013(7) -0.0032(6) -0.0042(7) O7 0.0204(7) 0.0427(11) 0.0263(8) 0.0050(8) 0.0108(6) -0.0021(7) O8 0.0375(10) 0.0201(8) 0.0299(9) 0.0066(7) 0.0050(7) 0.0085(7) O12 0.0167(6) 0.0130(6) 0.0125(6) -0.0017(5) -0.0004(5) 0.0009(5) O11 0.0158(6) 0.0127(6) 0.0114(6) 0.0001(5) 0.0005(5) 0.0011(5) O13 0.0174(7) 0.0205(7) 0.0119(6) -0.0010(5) 0.0012(5) 0.0012(6) O21 0.0107(6) 0.0148(6) 0.0155(6) -0.0023(5) -0.0008(5) -0.0004(5) O22 0.0111(6) 0.0235(8) 0.0193(7) -0.0101(6) 0.0012(5) -0.0003(5) O23 0.0179(7) 0.0215(7) 0.0173(7) -0.0053(6) 0.0016(5) -0.0032(6) N1 0.0127(7) 0.0115(7) 0.0126(7) -0.0006(6) 0.0013(5) 0.0000(6) N2 0.0158(8) 0.0130(8) 0.0250(9) -0.0057(7) -0.0057(6) 0.0031(6) N11 0.0148(7) 0.0128(7) 0.0128(7) 0.0000(6) 0.0000(6) -0.0002(6) N12 0.0169(7) 0.0140(8) 0.0126(7) 0.0020(6) 0.0017(6) 0.0000(6) N21 0.0118(7) 0.0143(7) 0.0137(7) 0.0000(6) 0.0013(5) -0.0005(6) N22 0.0132(7) 0.0179(8) 0.0160(7) -0.0003(6) 0.0031(6) -0.0030(6) N31 0.0120(7) 0.0141(7) 0.0151(7) 0.0007(6) 0.0008(6) -0.0002(6) N32 0.0110(7) 0.0174(8) 0.0177(8) 0.0028(6) 0.0008(6) 0.0006(6) N41 0.0203(8) 0.0117(7) 0.0138(7) 0.0001(6) -0.0006(6) 0.0004(6) N42 0.0290(9) 0.0158(8) 0.0148(8) -0.0008(6) 0.0006(7) -0.0016(7) N51 0.0217(8) 0.0128(8) 0.0217(8) -0.0036(6) -0.0061(7) 0.0064(7) N52 0.0239(9) 0.0145(8) 0.0240(9) -0.0046(7) -0.0039(7) 0.0081(7) N61 0.0123(7) 0.0115(7) 0.0181(7) -0.0020(6) 0.0044(6) -0.0021(6) N62 0.0148(7) 0.0119(8) 0.0317(9) -0.0031(7) 0.0098(7) -0.0030(6) C1 0.0104(7) 0.0151(9) 0.0147(8) -0.0005(7) 0.0011(6) 0.0007(6) C2 0.0129(8) 0.0129(8) 0.0195(9) -0.0044(7) 0.0012(7) -0.0001(7) C11 0.0203(9) 0.0172(9) 0.0145(8) -0.0003(7) -0.0003(7) -0.0019(7) C12 0.0290(11) 0.0165(9) 0.0146(9) -0.0003(7) 0.0046(8) -0.0010(8) C13 0.0241(10) 0.0181(10) 0.0175(9) 0.0063(8) 0.0018(7) 0.0020(8) C14 0.0266(10) 0.0141(9) 0.0233(10) 0.0047(8) 0.0027(8) 0.0020(8) C15 0.0200(9) 0.0140(9) 0.0177(9) 0.0003(7) 0.0005(7) 0.0015(7) C21 0.0184(9) 0.0142(9) 0.0195(9) 0.0006(7) 0.0026(7) -0.0016(7) C22 0.0190(9) 0.0141(9) 0.0238(10) -0.0004(7) 0.0049(8) -0.0029(7) C23 0.0130(8) 0.0319(12) 0.0218(10) -0.0021(9) 0.0047(7) -0.0054(8) C24 0.0135(8) 0.0339(12) 0.0201(10) -0.0033(9) 0.0041(7) 0.0019(8) C25 0.0146(8) 0.0213(10) 0.0182(9) -0.0017(8) 0.0029(7) 0.0030(7) C31 0.0174(9) 0.0200(10) 0.0230(10) -0.0038(8) 0.0049(7) 0.0032(8) C32 0.0144(8) 0.0155(9) 0.0276(10) 0.0003(8) 0.0011(7) 0.0026(7) C33 0.0106(8) 0.0278(11) 0.0221(10) 0.0071(8) 0.0002(7) -0.0016(8) C34 0.0164(9) 0.0258(11) 0.0297(11) 0.0055(9) -0.0009(8) -0.0072(8) C35 0.0180(9) 0.0176(9) 0.0225(10) 0.0002(8) 0.0010(7) -0.0048(8) C41 0.0277(11) 0.0284(12) 0.0235(11) 0.0034(9) -0.0010(9) -0.0019(9) C42 0.0309(12) 0.0411(15) 0.0223(11) -0.0140(10) -0.0065(9) 0.0101(11) C43 0.0413(14) 0.0287(12) 0.0192(10) -0.0007(9) 0.0124(9) -0.0074(11) C44 0.0301(12) 0.0355(13) 0.0269(11) 0.0000(10) 0.0143(9) -0.0088(10) C45 0.0206(9) 0.0211(10) 0.0203(9) 0.0028(8) 0.0045(8) -0.0045(8) C51 0.0198(10) 0.0297(12) 0.0345(12) -0.0033(10) 0.0020(9) 0.0019(9) C52 0.0241(10) 0.0179(10) 0.0289(11) -0.0013(8) 0.0027(9) 0.0044(8) C53 0.0349(13) 0.0144(10) 0.0311(12) -0.0053(9) -0.0023(10) 0.0088(9) C54 0.0367(13) 0.0142(10) 0.0329(12) -0.0054(9) -0.0059(10) 0.0026(9) C55 0.0262(11) 0.0150(10) 0.0291(11) -0.0044(8) -0.0086(9) 0.0029(8) C61 0.0239(11) 0.0253(11) 0.0305(12) 0.0009(9) -0.0011(9) -0.0046(9) C62 0.0172(9) 0.0184(10) 0.0501(15) 0.0025(10) 0.0085(10) -0.0007(8) C63 0.0255(10) 0.0133(9) 0.0293(11) 0.0001(8) 0.0116(9) -0.0022(8) C64 0.0247(10) 0.0139(9) 0.0264(10) 0.0045(8) 0.0035(8) 0.0008(8) C65 0.0150(8) 0.0142(9) 0.0208(9) 0.0029(7) 0.0022(7) -0.0001(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O11 1.8955(14) . ? Co1 O12 1.8977(14) . ? Co1 N31 1.9224(17) . ? Co1 N11 1.9254(17) . ? Co1 N21 1.9391(17) . ? Co1 N1 2.0113(17) . ? Co1 C1 2.320(2) . ? Co2 O22 1.8896(15) . ? Co2 O21 1.9062(14) . ? Co2 N61 1.9289(17) . ? Co2 N51 1.9348(18) . ? Co2 N41 1.9389(18) . ? Co2 N2 2.0085(17) . ? Co2 C2 2.322(2) . ? Cl1 O4 1.427(2) . ? Cl1 O2 1.4408(18) . ? Cl1 O1 1.4433(17) . ? Cl1 O3 1.4463(19) . ? Cl2 O7 1.4377(17) . ? Cl2 O5 1.4419(17) . ? Cl2 O6 1.4421(17) . ? Cl2 O8 1.4432(18) . ? O12 C1 1.319(2) . ? O11 C1 1.326(2) . ? O13 C1 1.230(2) . ? O21 C2 1.318(2) . ? O22 C2 1.327(2) . ? O23 C2 1.229(3) . ? N1 C11 1.502(3) . ? N1 C31 1.503(3) . ? N1 C21 1.511(3) . ? N2 C41 1.450(3) . ? N2 C61 1.532(3) . ? N2 C51 1.533(3) . ? N11 C15 1.339(3) . ? N11 N12 1.349(2) . ? N12 C13 1.350(3) . ? N12 C12 1.461(3) . ? N21 C25 1.342(3) . ? N21 N22 1.353(2) . ? N22 C23 1.346(3) . ? N22 C22 1.464(3) . ? N31 C35 1.339(3) . ? N31 N32 1.354(2) . ? N32 C33 1.348(3) . ? N32 C32 1.458(3) . ? N41 C45 1.335(3) . ? N41 N42 1.352(2) . ? N42 C43 1.344(3) . ? N42 C42 1.476(3) . ? N51 C55 1.335(3) . ? N51 N52 1.356(3) . ? N52 C53 1.354(3) . ? N52 C52 1.449(3) . ? N61 C65 1.337(3) . ? N61 N62 1.352(2) . ? N62 C63 1.341(3) . ? N62 C62 1.437(3) . ? C11 C12 1.506(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.376(3) . ? C13 H13 0.9300 . ? C14 C15 1.395(3) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C21 C22 1.505(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.378(3) . ? C23 H23 0.9300 . ? C24 C25 1.391(3) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C31 C32 1.512(3) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.379(3) . ? C33 H33 0.9300 . ? C34 C35 1.392(3) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C41 C42 1.514(4) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.375(4) . ? C43 H43 0.9300 . ? C44 C45 1.394(3) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C51 C52 1.517(3) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.366(4) . ? C53 H53 0.9300 . ? C54 C55 1.396(3) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C61 C62 1.489(4) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.374(3) . ? C63 H63 0.9300 . ? C64 C65 1.400(3) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Co1 O12 69.50(6) . . ? O11 Co1 N31 89.98(7) . . ? O12 Co1 N31 87.44(7) . . ? O11 Co1 N11 165.03(7) . . ? O12 Co1 N11 95.54(7) . . ? N31 Co1 N11 89.30(7) . . ? O11 Co1 N21 89.71(7) . . ? O12 Co1 N21 87.71(7) . . ? N31 Co1 N21 174.93(7) . . ? N11 Co1 N21 89.69(7) . . ? O11 Co1 N1 97.68(6) . . ? O12 Co1 N1 167.18(7) . . ? N31 Co1 N1 92.66(7) . . ? N11 Co1 N1 97.28(7) . . ? N21 Co1 N1 92.40(7) . . ? O11 Co1 C1 34.85(6) . . ? O12 Co1 C1 34.66(6) . . ? N31 Co1 C1 89.04(7) . . ? N11 Co1 C1 130.19(7) . . ? N21 Co1 C1 87.82(7) . . ? N1 Co1 C1 132.53(7) . . ? O22 Co2 O21 69.42(6) . . ? O22 Co2 N61 89.64(7) . . ? O21 Co2 N61 87.20(7) . . ? O22 Co2 N51 89.37(8) . . ? O21 Co2 N51 88.45(7) . . ? N61 Co2 N51 175.62(8) . . ? O22 Co2 N41 165.49(7) . . ? O21 Co2 N41 96.09(7) . . ? N61 Co2 N41 88.92(7) . . ? N51 Co2 N41 90.98(8) . . ? O22 Co2 N2 96.98(7) . . ? O21 Co2 N2 166.40(8) . . ? N61 Co2 N2 92.70(7) . . ? N51 Co2 N2 91.66(8) . . ? N41 Co2 N2 97.51(8) . . ? O22 Co2 C2 34.84(6) . . ? O21 Co2 C2 34.58(6) . . ? N61 Co2 C2 88.50(7) . . ? N51 Co2 C2 88.24(8) . . ? N41 Co2 C2 130.67(7) . . ? N2 Co2 C2 131.82(8) . . ? O4 Cl1 O2 110.49(15) . . ? O4 Cl1 O1 110.09(14) . . ? O2 Cl1 O1 109.32(11) . . ? O4 Cl1 O3 110.49(17) . . ? O2 Cl1 O3 108.91(11) . . ? O1 Cl1 O3 107.48(12) . . ? O7 Cl2 O5 109.28(11) . . ? O7 Cl2 O6 110.07(11) . . ? O5 Cl2 O6 108.63(11) . . ? O7 Cl2 O8 109.62(11) . . ? O5 Cl2 O8 109.73(11) . . ? O6 Cl2 O8 109.50(12) . . ? C1 O12 Co1 90.47(11) . . ? C1 O11 Co1 90.37(11) . . ? C2 O21 Co2 90.22(11) . . ? C2 O22 Co2 90.68(12) . . ? C11 N1 C31 108.08(16) . . ? C11 N1 C21 109.56(15) . . ? C31 N1 C21 105.91(16) . . ? C11 N1 Co1 111.59(12) . . ? C31 N1 Co1 115.06(13) . . ? C21 N1 Co1 106.40(12) . . ? C41 N2 C61 110.24(18) . . ? C41 N2 C51 110.53(19) . . ? C61 N2 C51 102.84(19) . . ? C41 N2 Co2 111.98(15) . . ? C61 N2 Co2 113.67(14) . . ? C51 N2 Co2 107.14(14) . . ? C15 N11 N12 106.46(16) . . ? C15 N11 Co1 126.06(14) . . ? N12 N11 Co1 127.28(13) . . ? N11 N12 C13 110.52(17) . . ? N11 N12 C12 121.43(16) . . ? C13 N12 C12 127.69(17) . . ? C25 N21 N22 106.17(16) . . ? C25 N21 Co1 125.61(15) . . ? N22 N21 Co1 127.99(13) . . ? C23 N22 N21 110.48(18) . . ? C23 N22 C22 125.29(19) . . ? N21 N22 C22 123.83(16) . . ? C35 N31 N32 106.12(16) . . ? C35 N31 Co1 129.60(15) . . ? N32 N31 Co1 123.55(13) . . ? C33 N32 N31 110.81(18) . . ? C33 N32 C32 129.83(18) . . ? N31 N32 C32 119.15(16) . . ? C45 N41 N42 106.56(18) . . ? C45 N41 Co2 126.14(15) . . ? N42 N41 Co2 126.17(15) . . ? C43 N42 N41 110.11(19) . . ? C43 N42 C42 128.0(2) . . ? N41 N42 C42 121.53(19) . . ? C55 N51 N52 106.18(18) . . ? C55 N51 Co2 125.07(15) . . ? N52 N51 Co2 127.78(16) . . ? C53 N52 N51 110.2(2) . . ? C53 N52 C52 126.4(2) . . ? N51 N52 C52 122.96(18) . . ? C65 N61 N62 106.20(17) . . ? C65 N61 Co2 129.22(14) . . ? N62 N61 Co2 123.25(13) . . ? C63 N62 N61 111.09(18) . . ? C63 N62 C62 128.35(19) . . ? N61 N62 C62 120.50(18) . . ? O13 C1 O12 125.90(19) . . ? O13 C1 O11 124.47(18) . . ? O12 C1 O11 109.63(16) . . ? O13 C1 Co1 178.03(16) . . ? O12 C1 Co1 54.87(9) . . ? O11 C1 Co1 54.78(9) . . ? O23 C2 O21 126.67(18) . . ? O23 C2 O22 123.67(19) . . ? O21 C2 O22 109.66(17) . . ? O23 C2 Co2 177.92(16) . . ? O21 C2 Co2 55.19(9) . . ? O22 C2 Co2 54.48(10) . . ? N1 C11 C12 114.52(17) . . ? N1 C11 H11A 108.6 . . ? C12 C11 H11A 108.6 . . ? N1 C11 H11B 108.6 . . ? C12 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? N12 C12 C11 113.47(18) . . ? N12 C12 H12A 108.9 . . ? C11 C12 H12A 108.9 . . ? N12 C12 H12B 108.9 . . ? C11 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? N12 C13 C14 107.69(18) . . ? N12 C13 H13 126.2 . . ? C14 C13 H13 126.2 . . ? C13 C14 C15 105.25(19) . . ? C13 C14 H14 127.4 . . ? C15 C14 H14 127.4 . . ? N11 C15 C14 110.07(19) . . ? N11 C15 H15 125.0 . . ? C14 C15 H15 125.0 . . ? C22 C21 N1 115.62(17) . . ? C22 C21 H21A 108.4 . . ? N1 C21 H21A 108.4 . . ? C22 C21 H21B 108.4 . . ? N1 C21 H21B 108.4 . . ? H21A C21 H21B 107.4 . . ? N22 C22 C21 115.16(17) . . ? N22 C22 H22A 108.5 . . ? C21 C22 H22A 108.5 . . ? N22 C22 H22B 108.5 . . ? C21 C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? N22 C23 C24 107.93(19) . . ? N22 C23 H23 126.0 . . ? C24 C23 H23 126.0 . . ? C23 C24 C25 105.10(19) . . ? C23 C24 H24 127.4 . . ? C25 C24 H24 127.4 . . ? N21 C25 C24 110.3(2) . . ? N21 C25 H25 124.8 . . ? C24 C25 H25 124.8 . . ? N1 C31 C32 114.74(17) . . ? N1 C31 H31A 108.6 . . ? C32 C31 H31A 108.6 . . ? N1 C31 H31B 108.6 . . ? C32 C31 H31B 108.6 . . ? H31A C31 H31B 107.6 . . ? N32 C32 C31 108.72(18) . . ? N32 C32 H32A 109.9 . . ? C31 C32 H32A 109.9 . . ? N32 C32 H32B 109.9 . . ? C31 C32 H32B 109.9 . . ? H32A C32 H32B 108.3 . . ? N32 C33 C34 107.31(19) . . ? N32 C33 H33 126.3 . . ? C34 C33 H33 126.3 . . ? C33 C34 C35 105.48(19) . . ? C33 C34 H34 127.3 . . ? C35 C34 H34 127.3 . . ? N31 C35 C34 110.3(2) . . ? N31 C35 H35 124.9 . . ? C34 C35 H35 124.9 . . ? N2 C41 C42 115.3(2) . . ? N2 C41 H41A 108.4 . . ? C42 C41 H41A 108.4 . . ? N2 C41 H41B 108.4 . . ? C42 C41 H41B 108.4 . . ? H41A C41 H41B 107.5 . . ? N42 C42 C41 115.7(2) . . ? N42 C42 H42A 108.4 . . ? C41 C42 H42A 108.4 . . ? N42 C42 H42B 108.4 . . ? C41 C42 H42B 108.4 . . ? H42A C42 H42B 107.4 . . ? N42 C43 C44 108.2(2) . . ? N42 C43 H43 125.9 . . ? C44 C43 H43 125.9 . . ? C43 C44 C45 104.8(2) . . ? C43 C44 H44 127.6 . . ? C45 C44 H44 127.6 . . ? N41 C45 C44 110.2(2) . . ? N41 C45 H45 124.9 . . ? C44 C45 H45 124.9 . . ? C52 C51 N2 113.4(2) . . ? C52 C51 H51A 108.9 . . ? N2 C51 H51A 108.9 . . ? C52 C51 H51B 108.9 . . ? N2 C51 H51B 108.9 . . ? H51A C51 H51B 107.7 . . ? N52 C52 C51 117.62(19) . . ? N52 C52 H52A 107.9 . . ? C51 C52 H52A 107.9 . . ? N52 C52 H52B 107.9 . . ? C51 C52 H52B 107.9 . . ? H52A C52 H52B 107.2 . . ? N52 C53 C54 107.9(2) . . ? N52 C53 H53 126.0 . . ? C54 C53 H53 126.0 . . ? C53 C54 C55 105.3(2) . . ? C53 C54 H54 127.3 . . ? C55 C54 H54 127.3 . . ? N51 C55 C54 110.4(2) . . ? N51 C55 H55 124.8 . . ? C54 C55 H55 124.8 . . ? C62 C61 N2 116.3(2) . . ? C62 C61 H61A 108.2 . . ? N2 C61 H61A 108.2 . . ? C62 C61 H61B 108.2 . . ? N2 C61 H61B 108.2 . . ? H61A C61 H61B 107.4 . . ? N62 C62 C61 108.2(2) . . ? N62 C62 H62A 110.1 . . ? C61 C62 H62A 110.1 . . ? N62 C62 H62B 110.1 . . ? C61 C62 H62B 110.1 . . ? H62A C62 H62B 108.4 . . ? N62 C63 C64 107.42(19) . . ? N62 C63 H63 126.3 . . ? C64 C63 H63 126.3 . . ? C63 C64 C65 105.44(19) . . ? C63 C64 H64 127.3 . . ? C65 C64 H64 127.3 . . ? N61 C65 C64 109.83(19) . . ? N61 C65 H65 125.1 . . ? C64 C65 H65 125.1 . . ? _diffrn_measured_fraction_theta_max 0.792 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.737 _refine_diff_density_min -0.932 _refine_diff_density_rms 0.098